反应详情

To a suspension of NaH (120 mg, 3 mmol, 60% in mineral oil) in dry THF (10 mL) at 0° C. under N2 atmosphere was added a solution of compound 7 (394 mg, 1.2 mmol) in dry THF (5 mL) and reaction mixture was allowed to stir for 30 min at room temperature. Compound 11 (300 mg, 1.2 mmol) in THF (2 mL) was then added and stirring was continued for 12 h at room temperature [reaction was followed by TLC]. Reaction mixture was quenched with water (5 mL), extracted with CH2Cl2 (40 mL), washed with brine, dried over Na2SO4 and concentrated. The crude mass was purified by column chromatography over silica gel using 10% methanol in chloroform as eluant to give 11a (110 mg, 28%) as pale yellow solid, mp 76.7-78.8° C.

1. additionwas added
2. stirringstirring
3. waitwas continued for 12 h at room temperature
4. custom[reaction was followed by TLC]
5. customReaction mixture
6. customwas quenched with water (5 mL)
7. extractionextracted with CH2Cl2 (40 mL)
8. washwashed with brine
9. dry with materialdried over Na2SO4
10. concentrationconcentrated
11. customThe crude mass was purified by column chromatography over silica gel using 10% methanol in chloroform as eluant