methyl 3,3,3-trifluoropropanoate

反応条件: temp:0.00; pressure:0.00; stir:

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: A solution of 150 g (1.5 mol) of potassium acetate in 500 ml of water was added dropwise to a solution of 105 g (0.5 mol) of methyl 2-(trifluoromethyl)-3,3,3-trifluoropropionate as above produced in 250 ml of water and the mixture was refluxed for 5 hours. After separation of the oily layer, extraction was made from the water layer that was left with use of methylene chloride and the solution of extracts and separated oily layer were joined and dried. After methylene chloride was removed by evaporation under atmospheric pressure, purification was made by distillation to give methyl 3,3,3-trifluoropropionate (TFPE) (54.07 g, 76%). Its analysis gave the following data: the mixture was refluxed for 5 hours After separation of the oily layer, extraction was left with use of methylene chloride the solution of extracts and separated oily layer dried After methylene chloride was removed by evaporation under atmospheric pressure, purification was made by distillation

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

実験手順: A solution of 3,3,3-trifluoro-propionic acid methyl ester (24.6 g, 173 mmol) in methanol (173 mL) was treated with hydrazine hydrate (8.4 mL, 173 mmol). The resulting mixture was then heated under reflux for 16 h and filtered. The filtrate was adsorbed on silica, evaporated and chromatographed (SiO2, dichloromethane:methanol=95:5 to 90:10). The title compound (14.2 g, 58%) was obtained as a white solid. MS: m/e=142.1 [M]+. The resulting mixture was then heated under reflux for 16 h filtered evaporated chromatographed (SiO2, dichloromethane:methanol=95:5 to 90:10)

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

実験手順: To a solution of 105 g (0.5 mol) of methyl 2-(trifluoromethyl)-3,3,3-trifluoropropionate in 250 ml of water, a solution of 150 g (1.5 mol) of potassium acetate in 500 ml of water was added dropwise and the mixture was refluxed for 5 hours. After separation of the oily layer, extraction was made from the water layer that was left using methylene chloride. The oily layer and extracted fraction were joined and dried. After evaporation of methylene chloride under atmospheric pressure, purification by distillation was performed to give methyl 3,3,3-trifluoropropionate (TFPE) (54.07 g, 76%). Its analysis gave the following data: the mixture was refluxed for 5 hours After separation of the oily layer, extraction was left The oily layer and extracted fraction dried After evaporation of methylene chloride under atmospheric pressure, purification by distillation