Nitric Acid → HCID 10866447, compound

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##

1. temperaturecooled to -30° to -40° C
2. extractionThe aqueous phase was extracted three times with 250 ml of dichloromethane
3. washthe combined organic phases were washed neutral with NaHCO3 solution and water
4. dry with materialdried with MgSO4
5. distillationdistilled
6. customAfter the solvent and first runnings (25 g; boiling range: 43°-98° C.) had been separated off

ORD record

ord-56dec003665a4dd59f8c99b3039cf5e7

Source dataset

uspto-grants-1984_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04459151