反应详情

To a slurry of intermediate 8 (77 mg, 0.23 mmol), 3-azetidinole hydrochloride (50 mg, 2 equiv.) and triethylamine (30 mL, 1 equiv.) in 20 mL of dichloromethane, was added NaBH(OAc)3 (146 mg, 3 equiv.) at room temperature. The reaction was stirred for 15 hour at room temperature and then quenched with 1N—NaOH. It was extracted with ethyl acetate and washed twice with brine. The collected organic layer was dried over anhydrous sodium sulfate and then concentrated in vacuo. The resulting residue was purified by recrystallization in a mixture of ethyl acetate and heptanes to afford desired Compound No. 140 as a pale yellow solid (62 mg, 69%); MS (ESI) m/z 390 [M+H]+.

1. customquenched with 1N—NaOH
2. extractionIt was extracted with ethyl acetate
3. washwashed twice with brine
4. dry with materialThe collected organic layer was dried over anhydrous sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe resulting residue was purified by recrystallization in a mixture of ethyl acetate and heptanes