反应详情

Dissolve (3-{[3-(4-chloro-pyridin-3-yl)-5-methyl-isoxazole-4-carbonyl]-amino}-cyclohexylmethyl)-carbamic acid benzyl ester (0.63 g, 0.0013 mol) in N,N-dimethylformamide (10 mL) at ambient temperature under a nitrogen atmosphere. Add a solution of potassium bis(trimethylsilyl)amide (0.5 M in toluene, 3.12 mL, 0.0016 mol) and stir for 15 min. at ambient temperature. Quench the dark mixture with water and follow by the addition of solid sodium chloride. Extract with ethyl acetate and wash the combined extracts with water and dry over sodium sulfate. Concentrate and elute over silica gel with methanol/dichloromethane to give 0.47 g (81%) of the desired product as a white solid. MS(ES): (M+1)+ 447.2, 448.2 m/z.

1. customQuench the dark mixture with water
2. additionfollow by the addition of solid sodium chloride
3. extractionExtract with ethyl acetate
4. washwash the combined extracts with water
5. dry with materialdry over sodium sulfate
6. concentrationConcentrate
7. washelute over silica gel with methanol/dichloromethane