反应详情

2 ml methyl lithium (1 M in diethylether) were added into a solution of 0.593 g 4,4-difluoro-cyclohexanecarboxylic acid methoxy-methyl-amide in anhydrous 5 ml THF at 0° C. The reaction was allowed to warm to rt overnight. The reaction was quenched with sat. ammonium chloride solution (˜50 ml) and diluted with sat. sodium hydrogencarbonate solution (25 ml). The aqueous layer was extracted with diethylether (3×50 ml) and the combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo. Purification was achieved by silica gel column chromatography (solvent: 5:1→1:1 petroleum/ether (40-60).

1. customThe reaction was quenched with sat. ammonium chloride solution (˜50 ml)
2. additiondiluted with sat. sodium hydrogencarbonate solution (25 ml)
3. extractionThe aqueous layer was extracted with diethylether (3×50 ml)
4. dry with materialthe combined organic phases were dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customPurification