ethyl 3,3,3-trifluoropropanoate

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 100 mL Hastelloy shaker tube was loaded with 26.5 g (0.227 mole) chlorosulfuric acid, cooled in liquid nitrogen, evacuated and loaded with 30 g (0.225 mole) of 1,1,3,3,3-pentafluoropropene. The reaction vessel was allowed to warm and kept on a shaker at 40° C. at autogenous pressure for 6 hours. The pressure tube was unloaded, and the reaction mixture was added drop by drop into the flask containing 60 ml of ethanol at −10° C. over a 15 minute period. The reaction mixture was stirred overnight at 20° C. and then was poured into 200 ml of ice water. The organic layer was separated, washed with sodium bicarbonate, water, and dried under MgSO4. Distillation gave 31 g of CF3CH2COOEt (87%), bp 108-109° C. cooled in liquid nitrogen evacuated to warm the reaction mixture was added drop by drop into the flask The organic layer was separated washed with sodium bicarbonate, water dried under MgSO4 Distillation

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 100 mL Hastelloy shaker tube was loaded with 26.5 g (0.227 mole) chlorosulfuric acid, cooled in liquid nitrogen, evacuated and loaded with 30 g (0.225 mole) of 1,1,3,3,3-pentafluoropropene. The reaction vessel was allowed to warm and kept on a shaker at 40° C. at autogenous pressure for 6 hours. The pressure tube was unloaded, and the reaction mixture was added drop by drop into the flask containing 60 ml of ethanol at −10° C. over a 15 minute period. The reaction mixture was stirred overnight at 20° C. and then was poured into 200 ml of ice water. The organic layer was separated, washed with sodium bicarbonate, water, and dried under MgSO4. Distillation gave 31 g of CF3CH2COOEt (87%), bp 108-109° C. cooled in liquid nitrogen evacuated to warm the reaction mixture was added drop by drop into the flask The organic layer was separated washed with sodium bicarbonate, water dried under MgSO4 Distillation

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

実験手順: Ethyl-3,3,3-trifluoropropanoate (2.5 g, 0.016 mol) and hydrazine monohydrate (1.2 g, 0.024 mol) were heated to reflux for 1 hour. The reaction mixture was concentrated under reduced pressure and the residue was treated with toluene (100 ml×3) to azeotrope hydrazine in excess. to reflux for 1 hour The reaction mixture was concentrated under reduced pressure the residue was treated with toluene (100 ml×3)

反応条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 100 mL Hastelloy shaker tube was loaded with 26.5 g (0.227 mole) chlorosulfuric acid, cooled in liquid nitrogen, evacuated and loaded with 30 g (0.225 mole) of 1,1,3,3,3-pentafluoropropene. The reaction vessel was allowed to warm and kept on a shaker at 40° C. at autogenous pressure for 6 hours. The pressure tube was unloaded, and the reaction mixture was added drop by drop into the flask containing 60 ml of ethanol at −10° C. over a 15 minute period. The reaction mixture was stirred overnight at 20° C. and then was poured into 200 ml of ice water. The organic layer was separated, washed with sodium bicarbonate, water, and dried under MgSO4. Distillation gave 31 g of CF3CH2COOEt (87%), bp 108-109° C. cooled in liquid nitrogen evacuated to warm the reaction mixture was added drop by drop into the flask The organic layer was separated washed with sodium bicarbonate, water dried under MgSO4 Distillation