1,1-二氟丙烷-1-烯

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1400 ml of hydrogen fluoride (anhydrous) and 320 g of nitric acid (concentrated) were initially introduced into a stirred steel autoclave and cooled to -30° to -40° C. 390 g (5 mol) of 1,1-difluoropropene were passed in at this temperature. The reaction mixture was allowed to warm up to room temperature, was further stirred for 6 hours, and was then poured onto 2 kg of ice. The aqueous phase was extracted three times with 250 ml of dichloromethane and the combined organic phases were washed neutral with NaHCO3 solution and water, dried with MgSO4 and distilled. After the solvent and first runnings (25 g; boiling range: 43°-98° C.) had been separated off, 615 g (=86% of theory) of 1-methyl-2,2,2-trifluoronitroethane [=1-(trifluoromethyl)nitroethane] were obtained; boiling point 98° to 100° C.; nD20 : 1.3380. ##STR17## cooled to -30° to -40° C The aqueous phase was extracted three times with 250 ml of dichloromethane the combined organic phases were washed neutral with NaHCO3 solution and water dried with MgSO4 distilled After the solvent and first runnings (25 g; boiling range: 43°-98° C.) had been separated off