反应详情

To a solution of [4-(methoxy-methyl-carbamoyl)-cyclohexyl]-carbamic acid tert-butyl ester (11 g, 38.4 mmol) in ether (200 mL), cooled to 0° C., was added MeMgBr (3M in ether, 32 mL, 96 mmol). The mixture was stirred 4 h at rt. 10% aq. NaHSO4 (200 mL) was carefully added. The two layers were decanted and the aq. layer was extracted with EA (100 mL). The combined org. layers were washed with brine, dried over Na2SO4, filtered and concentrated to dryness. The residue was purified by CC (Hept-EA 2:1), affording the title methyl ketone as a white solid (7.4 g, 80% yield).

1. customThe two layers were decanted
2. extractionthe aq. layer was extracted with EA (100 mL)
3. washlayers were washed with brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated to dryness
7. customThe residue was purified by CC (Hept-EA 2:1)