反应详情

温度

60 °C

A suspension of ethyl 4,4-difluorocyclohexanecarboxylate (2500 mg, 13 mmol) in ammonium hydroxide (28%, 50 ml) was stirred at 60° C. overnight. After removal of solvent, the residue was washed with water. The precipitate was obtained as product (white solid, 800 mg). 1H NMR (300 MHz, CDCl3): δ 5.31-5.45 (br, 2H), 2.02-2.27 (m, 3H), 1.92-2.02 (m, 2H), 1.72-1.87 (m, 4H). The mother liquor was acidified with 1N HCl to pH<1. The compound was extracted with EtOAc. The organic layer was washed with water, brine, dried over anhydrous sodium sulphate, filtered, condensed. 4,4-difluorocyclohexanecarboxylic acid was obtained as a 1200 mg of white solid which was further converted to 4,4-difluorocyclohexanecarboxamide by following procedure.

1. customAfter removal of solvent
2. washthe residue was washed with water
3. customThe precipitate was obtained as product (white solid, 800 mg)
4. extractionThe compound was extracted with EtOAc
5. washThe organic layer was washed with water, brine
6. dry with materialdried over anhydrous sodium sulphate
7. filtrationfiltered
8. customcondensed