funnel a mixture of 50 ml of bis [2(2-methoxyethoxy) ethyl] ether and 140 g of zinc dust, which had been treated with 100 ml of hydrochloric acid while suspended in acetone, filtered, and dried under vacuum for 4 h, was gently heated to about 60 °C with stirring. To this mixture was added 200 g (0.5 mol) of 4,6,7trichloroperfluoroheptene-1 with continued stirring. Heating was increased until refluxing was observed, then discontinued until addition was complete. The mixture was then gently refluxed for 1 h and permitted to cool to room temperature. The heptene and heptadiene were removed from the mixture by attaching a series of dry ice acetone-cooled traps to the condenser and applying a vacuum of less than 1 mm of mercury to the system. The solvent did not distill. The mixture of heptene and heptadiene was distilled at 75 mm. Three fractions were collected, between 35 and 45, between 45 and 50, and between 50 and 70 °C. A vapor-phase study showed the first fraction to be two-thirds heptadiene and two lower boiling components. The 45-50 fraction was almost pure heptadiene, while the 50-70 fraction contained small amounts of heptadiene and two higher boiling components. Above 70 °C virtually pure starting material was recovered. About 10 percent of the starting material remained in the solvent, and upon distillation of the solvent was converted into tar. Approximately 60 g of dechlorination products was estimated to be the desired heptadiene, or about 35 percent conversion on each dechlorination. The starting material was recycled.

The purest fraction obtained from distillation was run through a vapor-phase chromatograph and was found to contain trace amounts of all other dechlorination products. These trace materials were carefully removed through preparatory-scale vapor-phase chromatography before any attempt to polymerize or telomerize the compound was made. The pure heptadiene boiled at 112 °C/760 mm, which compares well with Park's 103°/633 mm.

2.2. Preparation of Perfluoropentadiene

Preparation of Sodium 3,5,6-Trichlorooctafluorohexanoate. In a 4-liter beaker, 320 g (8 mol) of sodium hydroxide was dissolved in 2 liters of water. The solution was vigorously stirred and 2915 g (8 mol) of 3,5,6richlorooctafluorohexanoic acid was added. The soluion became very viscous, but there was no precipitate. Chilling produced no precipitate, so the solution was poured into a clean vacuum desiccator and evaporated

near dryness by using an infrared lamp and an aspiator. The salt became syrupy, buttery, and then waxy. ut did not crystallize. The salt was then dried at 10-2 am (dry ice acetone trap) for three days. Water (500 l) was removed, and the wax became a white, crystalne material. Drying was continued for two more days, ith removal of water (200 ml), and the crystals became fine. apparently amorphous, rather hygroscopic

owder.

3,5,6-Trichlorooctafluoro

Pyrolysis of Sodium hexanoate. 3,5,6-Trichlorooctafluorohexanoate (2.2 kg) was pyrolyzed under reduced pressure in a stainless steel tube connected, through adapters, to a series of cooled traps (dry ice acetone) and heated to approximately 350 °C in a furnace controlled by two 10 A, variable transformers. Pyrolysis took place smoothly, yielding 1520 g of products (theoretical yield, 1600 g). This was 95 percent based on the salt. The product was carefully distilled through a 10-in glass column packed with glass helices. A fraction boiling at 91 °C was collected as the desired product. It amounted to 1360 g (85%. based on the acid salt).

ANAL. Caled. for CCF: C, 21.2%; Cl, 25.1%; F, 53.7%. Found: C, 21.0%; Cl, 24.8%.

In the same distillation, a second fraction was obtained, boiling at 120 °C. This amounted to 145 g (9% based on the acid salt). The remaining material would not distill at atmospheric pressure, and was assumed to be a coupling product. No further effort was made to characterize it. The 120 °C fraction showed three peaks on a gas-liquid chromatogram, and a deep, split band between 5 and 6 μ in its infrared spectrum. This appeared to be a mixture of the isomers of trichloroheptafluoropentene. This was supported by the elemental analysis and by conversion into a mixture of a three monochloroheptafluoropentadienes.

ANAL. Calcd. for CCF7: C. 20.3%; Cl, 35.2%. Found: C, 20.1%; Cl, 34.9%.

Dechlorination of 4,5-Dichlorooctafluoro-1-pentene. Dechlorination was effected by a slight variation of the method of Park and Lacher [4]. In a beaker, 130 g (2.0 mol) of powdered zinc was suspended in acetone, and 100 ml of concentrated hydrochloric acid was added slowly with stirring. Stirring was continued for 30 min. The zinc was filtered off with suction, washed thoroughly with acetone, dried briefly in air, and then overnight in a vacuum oven at 70 °C. This activated zinc was placed in a 500-ml, three-necked flask (equipped with an efficient stirrer, a dropping funnel, and a 6-in glass column packed with glass helices and topped by a still-head) and 200 ml of bis[2-(2-methoxyethoxy)ethyl] ether was added. Stirring was commenced, and the flask was heated (Thermowell heater) to 70 °C. 4,5-Dichlorooctafluoro-1-pentene (284 g, mol) was added in small portions until the reaction started, and then dropwise until addition was complete, Perfluoropentadiene distilled out of the column at about the same rate as the pentene was added. The rate of addition of the pentene and the heat applied to the flask were so controlled that the temperature of the distillate never exceeded 40 °C. The yield of crude pentadiene was 194 g (91%); this was distilled through a 10-in glass column, packed with glass helices, yielding a pure product, boiling at 36 °C, that showed one major peak (and two minor peaks with 1% and 0.3% of the area of the major peak) on an analytical gas-liquid chromatogram. The yield of pure compound was 160 g (89%). Recovered starting material (34 g) was recycled. Its infrared spectrum showed a single band at 5.6 μ, the band being somewhat broader and more intense

ANAL. Calcd. for C5F8: C, 28.3%; F, 71.7%. Found: C, 28.1%; F, 70.9%.

Dechlorination of Trichloroheptafluoropentene Fraction. The dechlorination procedure described for the preparation of perfluoro-1.4-pentadiene was repeated. A 60 g (0.2 mol) portion of the trichloroheptafluoropentene fraction was added to the flask containing the high-boiling ether and activated zinc. During the dechlorination, the distillate came over below 70 °C. The crude yield was 42 g or 92%. Upon careful distillation at 65 °C, 39 g of a mixture of monochloroheptafluoropentadienes was obtained, which was 85 percent based on the pentene; 5 g of starting material was recovered and recycled.

ANAL. Calcd. for C5CIF7: C, 26.3%; Cl, 15.5%; F, 58.2%. Found: C, 26.6%; Cl, 15.2%; F, 58.1%.

2.3. Telomer Studies

Addition of Iodine Monochloride to Trifluoroethylene. In an 800-ml stainless steel bomb 238 g (2.9 m) of trifluoroethylene and 454 g (2.8 m) of iodine' monochloride were shaken for 24 h at room temperature. The small excess of the ethylene was permitted to escape. The yield was 650 g of material boiling at 84 °C or 95 percent based on iodine monochloride.

Addition of Iodine Monochloride to Tetrafluoroethylene. In an 800-ml stainless steel bomb 100 g (1 m) of tetrafluoroethylene and 162 g (1 m) of iodine monochloride was shaken at room temperature for 24 h. The contents were removed from the bomb, shaken with aqueous sodium bisulfite, dried over anhydrous sodium sulfate and distilled. The yield was 200 g of clear liquid boiling at 56 °C or 76.5 percent based on either reagent.

Addition of Iodine to Tetrafluoroethylene. In a 1400ml bomb was placed 254 g (1.0 m) of I2 and 210 g (1.0 m) of CF2Br2. Through a vacuum line 100 g (1.0 m) of tetrafluoroethylene was distilled into the bomb. The bomb and its contents were rocked for 2 days at room temperature without diminution of pressure. The temperature was raised to 100° for 16 h and shaking was continued. The bomb was cooled to room temperature and the internal pressure was found to have decreased from 150 psi to atmospheric. A solution weighing 450 g was transferred from the bomb to a distilling flask. From this solution 140 g of dibromodifluoromethane and 40 g of iodine were recovered. The product, 1,2-diodotetrafluoroethane amounted to 210 of a purple liquid boiling at 112 to 113 °C or 62.1 percent based on the tetrafluoroethylene.

Addition of Iodine Monochloride to Chlorotrifluoroethylene. A 12-liter three-neck flask equipped with a stirrer and dropping funnel was placed in a constant temperature bath set at -10 °C and fastened securely. Into it was poured 5000 ml of clean dry methylene chloride. Dropwise 2500 g 15.4 mol of iodine monochloride was added. The dropping funnel was replaced with a dry ice acetone-cooled condenser.

trifluoroethylene was distilled directly from the cylin der. Stirring and gentle refluxing of the ethylene was continued for six weeks. The flask was then removed from the bath and permitted to warm to room temperature. The unreacted ethylene was distilled into a dry ice acetone-cooled trap and saved for the next run. The contents of the flask were removed, the methylene chloride distilled and the product was fractionated through a 10-in column packed with helices. The forecut consisted of two fractions boiling at 46 °C and 54 °C. The desired product, CF2CICFCII, boiling at 101 °C amounted to 3100 g or 72.6 percent based on the iodine monochloride which was not chemically pure. A considerable quantity of iodine remained in the reaction flask.

Addition of Iodine Monochloride to Chlorotrifluoroethylene. In a 1400-ml steel bomb was placed 1000 g (6.2 m) of technical grade iodine monochloride. The bomb was cooled to -196° using liquid nitrogen and into it was distilled 727 g (6.25 m) of chlorotrifluoroethylene. The bomb was permitted to warm to room temperature while rocking. It was then rocked for 65 h at room temperature. At the end of this period the contents were removed, shaken with aqueous sodium bisulphite and dried over anhydrous sodium sulfate. The amount of crude product was 1510 g or 88 percent based on the impure iodine monochloride. Distillation produced a forecut boiling below 50 °C and 1415 g of product boiling at 101 °C or 82.5 percent based on iodine monochloride. This product was found to be a mixture of isomers CF CICFCII and CF2ICFC12. but was largely the latter.

Telomerization of 1-Chloro-1,1.2-trifluoro-2-iodoethane with Tetrafluoroethylene. A glass tube containing 47.6 g (0.2 m) of CFCICFHI and 20 g (0.2 m) of CF CF2 was subjected to ordinary room light for a brief period at 0 °C. Upon warming to 0° from - 196 °C solid polymer began forming immediately. After all action had apparently ceased the tube was opened and any remaining CF CF was permitted to escape. Resolution of the mixture yielded 33 g of the starting ethane, 3 g of very high boiling viscous liquid product and 5 g of solid polymer, both assumed to be low molecular weight polytetrafluoroethylene. Telomerization of 1-Chloro-tetrafluoro 2-iodoethane with Tetrafluoroethylene. A glass tube charged with 49.6 g (0.19 m) of CF2ICF2Cl and 18.8 g (0.19 m) of CF2CF2 was permitted to warm from 195 °C to room temperature. It was subjected to ordinary fluorescent light for 8 h at room temperature then opened. Separation of the components of this mixture. yielded 35 g of original ethane 3 g of material boiling between 60° and 120 °C and 11 g of polymer. Excess ethylene again was permitted to escape.

Telomerization of tetrafluoro 1,2-Diiodoethane with Tetrafluoroethylene. A glass tube containing 65.4 g (0.184 m) of CFICFI and 18.4 g (0.184 m) of CFCF was subjected for three days to radiation from a cobalt 60 source at a dose rate of 0.25 megarads/h. The yields were as follows:

Telomerization of 1,2-Dichlorotrifluoro-1-iodoethane with Tetrafluoroethylene. Into a thick-walled glass tube containing 500 g (1.8 m)CFCICFCII was distilled 192 g (1.9 m) of CF CF2. The tube was thoroughly degassed and placed in a cobalt-60 source where it was subjected to a dose rate of 0.25 megorads/h for 20 h. It was then cooled to 196 °C with liquid nitrogen and opened. On warming to room temperature excess tetrafluoroethylene was permitted to escape. The liquid mixture was transferred to a distilling flask and distilled, first roughly then carefully through a 10-in column packed with glass helices. The yields of telomers were as follows:

99-101°

101-140°

Telomerization of 1,2-Dichloro-heptafluoro-4-iodobutane with Hexafluoropropylene. Into a 1400-ml bomb was placed 760 g (2 mm) of 1,2-dichloro-4-iodoheptafluorobutane. The bomb was attached to a vacuum line cooled to - 195 °C and evacuated. Into it was distilled 470 g (3.14 m) of carefully degassed hexafluoropropylene. The bomb was sealed, placed in a heaterrocker mechanism, heated to 202 °C and rocked at this temperature for 411 h. It was then cooled to room temperature and attached to a dry ice acetone-cooled trap. In this way about 50 g of impure hexafluoropropylene was recovered. Total amount of liquid (or solid) product was 1071 g. The liquid was distilled roughly under reduced pressure giving the following yields. 546 g

< 130°/20 mm

CF CICFCH(CF2I higher telomers

Telomerization of 1,2-Dichloro-trifluoro-1-iodoethane with Hexafluoropropylene. Into a 1400-ml bomb was oured 560 g (2 m) of 1,2-dichloro-1-iodotrifluoroethane. The bomb was attached to a vacuum line cooled to -196 °C and evacuated. Into it was distilled 800 g 5.3 m) of carefully degassed hexafluoropropylene. The bomb was sealed and placed in a heater-rocker ssembly, heated to 200°, and rocked at this temperaure for 294 h. It was then cooled to room temperature nd 210 g of excess hexafluoropropylene was distilled to a dry ice-acetone cooled trap. The liquid product. 10 g of a dark oil was distilled and the following

Preparation of 1,5,6-Trichloroperfluorohexane. In each of two quartz tubes was placed 67 g (0.14 m) of CF CICFCI(CF), and 28.4 g (0.4 m) of chlorine. The tubes were shaken and irradiated with ultraviolet light from a Hanovia type L burner for 13 h. The tubes were opened and the excess chlorine permitted to escape. The liquid mixtures were combined and distilled. The amount of desired product was 65 g or 61.8 percent conversion. Thirty nine grams of iodocompound were recovered unchanged. Taking this into consideration the yield was 84.1 percent. A small residue was not identified. Boiling point of the slightly impure material was 146 °C.

Dehalogenation of 1,5,6-Trichloroperfluorohexane. In a 1-liter flask equipped with a still head and stirrer 61 g (0.17 m) of CF2CICFCl(CF2),Cl, 60 g (0.9 m of Zn 90 ml of acetic anhydride and 270 ml of acetic acid was stirred and heated to 90°. The 6-chloroperfluoro-1hexane distilled. The crude product was washed with water, dried over anhydrous sodium sulfate and redistilled. Yield of pure product was 27 g or 54 percent B.P. 89°.

Attempted Dechlorofluorination of 6-Chloroperfluoro-1-hexene. In a 1-liter flask equipped with a stirrer, reflux condenser, and a thermometer extending into the liquid were placed 30 g (0.09 m) of CFCF(CF)Cl. 13 g (0.2 m) of Zn and 200 ml of diethylene glycol. The mixture was stirred and heated to 140 °C, the hexane refluxing vigorously. At 140° the contents of the flask began to seethe and froth and the refluxing subsided. No further reflux was observed until the temperature reached 190°. The reflux condenser was replaced with a still head and a product was distilled at 182 °C. This is the B.P. that Knunyants has reported for perfluoro-1.11-dodecadiene. The yield was 13 g or 50 percent.

added dropwise an intimate mixture of 556 g (2m) 1,2-dichloro-trifluoro-1-iodoethane and 760 g (2m) of 1,2-dichloro-4-iodoperfluorobutane. During the addition of the halocarbon mixture reflux was maintained without application of external heat. When addition was complete reflux and stirring were continued overnight. The contents of the flask were filtered and the residue discarded. The filtrate was added slowly with stirring to 5000 ml of water in two 4-liter beakers. The aqueous layer was discarded. The methylene chloride solution was dried over anhydrous sodium sulfate and distilled. It was then redistilled through an 18-in column packed with glass helices with the following results.

These tubes were shaked and irradiated with ultraviolet rays from a Hanovia Type L burner for 35 h. The contents of the tubes were combined and the organic material was carefully separated from the mercury and distilled. The yield was 34 g of material, boiling at 68 °C/3 mm or 68.5 percent based on the fluorocarbon, since 40 g of fluorobutane was recovered.

(Knunyant's Method)

In a 250-ml 3-neck flask, complete with stirrer. reflux condenser and dropping funnel, was placed a mixture of 10 g (0.15 m) of powdered zinc in 31 g of acetic anhydride and 50 ml of methylene chloride. This mixture was stirred vigorously and heated to reflux. To it was added dropwise 57 g (0.15 m) of CF CICFCICF CFI. During the addition, heating was discontinued but a vigorous reflux was maintained by the rate of addition. After addition, heating was resumed and reflux was maintained for 6 h. The flask was cooled and its contents were filtered and added dropwise to 1 liter of water. The organic layer was separated, dried over anhydrous sodium sulfate and distilled. Careful distillation thorugh a 10-in column packed with glass helices yielded 22.4 g of a clear colorless liquid boiling at 68 C/3 mm. This was 59.3 percent based on the dichloroiodoperfluorobu

tane.

Cross-coupling of 12-Dichlorotrifluoro-1-iodoethane and 12-Dichloro-perfluoro 4-iodobutane. Into a 3-liter. 3-neck flask equipped with a stirrer reflux condenser and dropping funnel was placed a mixture of 260 g (4.0 m) of zine powder, 800 ml of acetic anhydride and 2000 ml of methylene chloride. This mixture was stirred and heated to reflux. To this refluxing mixture was

1.2.7.8-Tetrachloroperfluorooctane.

Residue.......

> 68/1 mm 210

Preparation of 7,8-Dichloroperfluorooctanoic Acid Thirty g (0.05 m) of 1,2-dichloro-8-iodoperfluorooctane and 20 ml of 60 percent oleum were placed in a 100 m2 steel bomb and the bomb sealed. The bomb was rocked and maintained at 250 °C for 18 h. The contents were removed from the bomb. The oily organic layer was separated and shaken with aqueous sodium bicarbonate until neutral to pH paper. The solution was ther made acidic with dilute surfuric acid and extracted continuously with ether. The ether extract was drie: over anhydrous sodium carbonate and distilled. The yield was 9.4 g of a colorless oil boiling at 155°/58 mm This was 38 percent based on the iodooctane used as starting material. On standing the oil slowly solidified This was consistent with the findings of Knunyants This acid was later converted to the sodium salt and the salt dried by conventional means.

Preparation of Sodium 7,8-Dichloroperfluorooctano ate. A mixture of 145 g (0.25 m, 73 ml) of 7,8-dichlore 1-iodoperfluorooctane and 291 g (2.5 m 173 mb of chlorosulfonic acid was placed in a glass tube of suce size that the tube was about 3 full. The tube was placed in a metal bomb surrounded with carbon tetra chloride. The bomb was sealed and placed in a heater The heater was inclined so that the glass tube was about 85° from vertical. The bomb and contents were maintained at 146-152° for 20 h after which the bot was permitted to cool to room temperature. The glass tube was removed and cooled to 196 °C with liqu nitrogen. It was opened and permitted to warm to roor temperature. Warming was accelerated by pourin warm water over the outside of the tube. The contentof the tube was poured on ice cubes. During this str most of the ice melted. On standing an oily layer sepa rated. The aqueous layer was decanted. The oily lave amounting to 127 g, was added dropwise to a hot so tion of 40 g (1.0 m) of sodium hydroxide in 500 ml

water After addition, heating was continued for two hours. The mixture was ther permitted to coo to room temperature and retrigerated overnight. The crystais of 16-arta-roperfiurocanviate were filtered and vacuzzi, cred. The vieid was tit g or 56.3 percent based on the a Compound From the nitrate 35 £ ot oi was obtained. This was subverted to intrared analysis and was esencruded to be 1.7.&trichioroperfluoroheptane which Hauptschier, suggested to be a byproduct in this type i reation. The reaction was carried out six times with the virias varving between 4 and 56.5 percent. The product is a white microcrystalline

materia

Preparat in or 14-1st.oropentafluorobutyric Arid. In a 2-liter. S-nek fiask equipped with an efficient stirrer and & on stem thermometer, a mixture of 273 g165 m £ potassium permanganate. 350 ₫ 4.2 m2 ot sodium tocar mate. 100 mi of acetone and 400 m. of water was stired and cooled to 4 C. To this mixture was added in gwise 284 £ 10 m of

COFC CIFCF, CF=CF

The latter compound was obtained from the pyrolysis of CCF_CC_FCF_CFGCF.COON= in a manner de scribed in earder work 15. After addition the mixture was permitted to warm slows to room temperature. care being exercised to prevent excessive foaming. Excess permanganate was destroyed with 5 percent aqueous sodium bisulphite. Manganese dioxide thus formed was titered, washed with water, and discarded. The combined nitrate and wastings were clear and colorless. To this was added 100 m 244 c. 5 m of 95 percent sufuric acid. This acid solution was extracted continuous, with ether for 50 h. The extract was dried over anhydrous odium sulphate and distilled. The product was dist Jed under reduced pressure, vieiding 121 g of a clear, cu mess o, boiling at 100 °C. 3 mm. This was 49 percent based or the pentene

Preparation of 3,4-Diet oropentafluorobutyric Acid Alternative Preparation Into a 5-iter. 3-neck flask equipped with a condenser arranged for downward dis tillation was placed 570 g 15 m 2 CCF.CCFCF;CF;I and 2000 g of 20 percent fuming sulfuric aod. This mixture was heated gents unt the add fluoride, (

CCIF CCIFCF-C-F. bezen to dist!! Heating was then carefully adjusted so that the acid foonde would continue to distill with a minimum of impurities. Sultur trioxide which was evoved or copious quantities during the addition was vented from the system through a tube attached to an adapter between the condenser and the receiver. The crude acid fluoride-jodobutane laver. 283 g. was shaken with cont sulünc acid in a separatory funnel. removing dissolved sutur trodde, then disc tilled through a column The yed was 158 g of

CCIF.CCIFCF.C-F. A;:exmates 107 g of butane was recovered. The yield of acid fluoride was 52.3 percent based on the god butane, which reacted.

The acid fluoride was added dropwise to a solutior ot 80 g at sodium hydroxide 11. 200 m. of water. The mixture was heated to 90 °C and maintained at this temperature for 30 min 1: was cooled and a smai amount of of separated The aqueous alkal solution was acidified with. 50 percent sulfuric acid and extracted continuous'x with ether for five days. The ether extract was dried over ant ydrous sodium sultate and distilled The product. 3,4-dichloropentafluorobutyric acid was obtained by distiliation under reduced pressure t amounted to 149 got a clear colorless homɑ boiling at 100 5 mm. This was 95 percent based on the acic fluoride or 495 percent based or the jodobutane

Preparation of 54-chich oropen'a fiu:orobutyric 4riá Ind A. ternative Preparation. In a stainless stee homb was placed 152 40.5 m. 76 ml of 1.1.3.4-tetrachlorohexafluorobutane 5M Ke÷F Dimet No. 404 72 m2 ot cone, sufuric acid and 34 m: of 30 percent fuming Sulturic acid. The bomb was seated. It was rocked. heated to 200 °C and maintained at this temperature for 96 h. It was cooled to− 80 °C, opened and permitted to warm to room temperature. Intense foaming and evolution, of gas occurred, but the contents of the bombs were successfully transferred to a beaker On standing, the foaming and gas evolution subsided. This mixture was distilled under reduced pressure vieiding 65 g of clear liquid boiling at 67° 1 mm or 53 percent based on the butane It gave the same index of revaction as samples prepared in the other two ways. \, 1.3470.

Preparation of 3-Chloropentafluoropropene. Fitty rams (0.21 m) of 3,4-dichloropentafluorobutyric acid were converted to the sodium salt by neutralizing ar aqueous solution of the acid with sodium hydroxide so that the resulting solution had a pli of 7. This was evaporated to absolute dryness in a vacuum, desiccatot, vieiding 56 g of anhydrous sodium 3,4-dichloropeniafluorobutyrate The salt was pyrolyzed in a 250 m. round-bottom flask which was connected by adapters to three liquid nitroger-cooled traps connected in tandem. Heat was supplied by a microburner The vieid was 32 g or 91.5 percent based on the acid salt This was distified through a column packed with glass helices. The yield of pure compound was 30 g or 862 percent. RP. 8°C.

Preparation of Pentafuoro 3-lodopropene. A 2-liter, 3-neck flask was equipped with a stirrer, a thermometer, and a reflux condenser topped by a dry ice acetone-cooled onld finger type condenser topped by a calcium chloride drying tube Into the Sask was piaced 83 g 06 m of sodium iodide and 300 m. of trestov distilled methylethy ketone Stirring was commenced and into the flask was dist red 58 g 0.35 m of 3chaoropentafla in propene. The mature was relaxed for 24 h. The reflux tem perature rose from 20 to 60 °C. The product was removed from the flask, filtered, and the trate distled. A fract or boring between 50° and 55 was c ected and redist Led through a léir co amn parked with gass heaves. The vicd was 40 g of a crat Conor Uss Lelid which słów ▼ turned visit on stand ne

This was 442 percent based on the chloropentafiaoroPropene B.P, 55 °C.

408-434 - 71 - 4