(2-chloro-2,2-difluoroacetyl) 2-chloro-2,2-difluoroacetate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a clean dry 600 mL Parr pressure reactor was charged 53.5 g (0.92 mol) of anhydrous potassium fluoride, 150 g of anhydrous diglyme and 150 g of chlorodifluoroacetic anhydride. With the reactor set at 80° C. and 92 psig (5500 torr), 123 g (0.820 mol) of hexafluoropropylene was charged over a 3 hour period at a tank pressure not exceeding 120 psig (7000 torr). Following reaction for ½ hour at 80° C., the reactor contents were allowed to cool and were distilled to obtain 180.6 g of crude material. Upon fractional distillation, acetic acid/KMnO4 treatment and refractionation of the crude material, 46.1 g (26% of theoretical yield) of (CF3)2CFC(O)CF2Cl, a clear colorless liquid, was obtained having a purity of 98.8% as determined by gas chromatography. To a clean dry 600 mL Parr pressure reactor set at 80° C. reaction for ½ hour at 80° C. to cool were distilled

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a clean dry 600 mL Parr pressure reactor was charged 53.5 g (0.92 mol) of anhydrous potassium fluoride, 150 g of anhydrous diglyme and 150 g of chlorodifluoroacetic anhydride. With the reactor set at 80° C. and 92 psig (5500 torr), 123 g (0.820 mol) of hexafluoropropylene was charged over a 3 hour period at a tank pressure not exceeding 120 psig (7000 torr). Following reaction for ½ hour at 80° C., the reactor contents were allowed to cool and were distilled to obtain 180.6 g of crude material. Upon fractional distillation, acetic acid/KMnO4 treatment and refractionation of the crude material, 46.1 g (26% of theoretical yield) of (CF3)2CFC(O)CF2Cl, a clear colorless liquid, was obtained having a purity of 98.8% as determined by gas chromatography. To a clean dry 600 mL Parr pressure reactor set at 80° C. reaction for ½ hour at 80° C. to cool were distilled

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a clean dry 600 mL Parr pressure reactor was charged 53.5 g (0.92 mol) of anhydrous potassium fluoride, 150 g of anhydrous diglyme and 150 g of chlorodifluoroacetic anhydride. With the reactor set at 80° C. and 92 psig (5500 torr), 123 g (0.820 mol) of hexafluoropropylene was charged over a 3 hour period at a tank pressure not exceeding 120 psig (7000 torr). Following reaction for ½ hour at 80° C., the reactor contents were allowed to cool and were distilled to obtain 180.6 g of crude material. Upon fractional distillation, acetic acid/KMnO4 treatment and refractionation of the crude material, 46.1 g (26% of theoretical yield) of (CF3)2CFC(O)CF2Cl, a clear colorless liquid, was obtained having a purity of 98.8% as determined by gas chromatography. To a clean dry 600 mL Parr pressure reactor set at 80° C. reaction for ½ hour at 80° C. to cool were distilled

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a clean dry 600 mL Parr pressure reactor was charged 53.5 g (0.92 mol) of anhydrous potassium fluoride, 150 g of anhydrous diglyme and 150 g of chlorodifluoroacetic anhydride. With the reactor set at 80° C. and 92 psig (5500 torr), 123 g (0.820 mol) of hexafluoropropylene was charged over a 3 hour period at a tank pressure not exceeding 120 psig (7000 torr). Following reaction for ½ hour at 80° C., the reactor contents were allowed to cool and were distilled to obtain 180.6 g of crude material. Upon fractional distillation, acetic acid/KMnO4 treatment and refractionation of the crude material, 46.1 g (26% of theoretical yield) of (CF3)2CFC(O)CF2Cl, a clear colorless liquid, was obtained having a purity of 98.8% as determined by gas chromatography. To a clean dry 600 mL Parr pressure reactor set at 80° C. reaction for ½ hour at 80° C. to cool were distilled

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: tert-Butyl[1-(3,4-dichlorophenyl)-1-methylaminomethyl-3-butenyl]methylcarbamate (500 mg) produced in Example 4 was dissolved in methylene chloride (10 mL). Under cooling with ice, pyridine (163 μL) and chlorodifluoroacetic acid anhydride (350 μL) were added thereto. Under cooling with ice, the mixture was stirred for 50 minutes. Saturated aqueous sodium bicarbonate was added to the reaction mixture, and the resultant mixture was extracted with methylene chloride. The organic layer was washed with saturated brine, dried over sodium sulfate anhydrate, and concentrated under reduced pressure. The residue was purified through silica gel column chromatography (n-hexane:ethyl acetate=4:1), to thereby give the title compound (300 mg, 46%). were added Under cooling with ice the resultant mixture was extracted with methylene chloride The organic layer was washed with saturated brine dried over sodium sulfate anhydrate concentrated under reduced pressure The residue was purified through silica gel column chromatography (n-hexane:ethyl acetate=4:1)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a clean dry 600 mL Parr pressure reactor was charged 53.5 g (0.92 mol) of anhydrous potassium fluoride, 150 g of anhydrous diglyme and 150 g of chlorodifluoroacetic anhydride. With the reactor set at 80° C. and 92 psig (5500 torr), 123 g (0.820 mol) of hexafluoropropylene was charged over a 3 hour period at a tank pressure not exceeding 120 psig (7000 torr). Following reaction for ½ hour at 80° C., the reactor contents were allowed to cool and were distilled to obtain 180.6 g of crude material. Upon fractional distillation, acetic acid/KMnO4 treatment and refractionation of the crude material, 46.1 g (26% of theoretical yield) of (CF3)2CFC(O)CF2Cl, a clear colorless liquid, was obtained having a purity of 98.8% as determined by gas chromatography. To a clean dry 600 mL Parr pressure reactor set at 80° C. reaction for ½ hour at 80° C. to cool were distilled

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a clean dry 600 mL Parr pressure reactor was charged 53.5 g (0.92 mol) of anhydrous potassium fluoride, 150 g of anhydrous diglyme and 150 g of chlorodifluoroacetic anhydride. With the reactor set at 80° C. and 92 psig (5500 torr), 123 g (0.820 mol) of hexafluoropropylene was charged over a 3 hour period at a tank pressure not exceeding 120 psig (7000 torr). Following reaction for ½ hour at 80° C., the reactor contents were allowed to cool and were distilled to obtain 180.6 g of crude material. Upon fractional distillation, acetic acid/KMnO4 treatment and refractionation of the crude material, 46.1 g (26% of theoretical yield) of (CF3)2CFC(O)CF2Cl, a clear colorless liquid, was obtained having a purity of 98.8% as determined by gas chromatography. To a clean dry 600 mL Parr pressure reactor set at 80° C. reaction for ½ hour at 80° C. to cool were distilled