反应详情

To a stirred suspension of Compound 7 (1.25 g, 7.66 mmol) in CH2 Cl2 (40 ml) was added acetic anhydride (860 mg, 8.42 mmol) and triethylamine (2.32 g, 22.98 mmol) at room temperature. The reaction mixture was stirred at room temperature for 22 h. The mixture was diluted with H2O (50 ml) and stirred for 10 min. The organic layer was separated and the aqueous layer was extracted with CH2Cl2. The combined solution was washed with 10% HCl aq., sat. NaHCO3 aq. and brine, dried (MgSO4) and concentrated in vacuo to give crude product (1.58 g, quant.), which was recrystallized from hexane-ethyl acetate to give Compound 8 (1.26 g, 80%) as a white solid.

1. stirringstirred for 10 min
2. customThe organic layer was separated
3. extractionthe aqueous layer was extracted with CH2Cl2
4. washThe combined solution was washed with 10% HCl aq., sat. NaHCO3 aq. and brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. customto give crude product (1.58 g, quant.), which
8. customwas recrystallized from hexane-ethyl acetate