反应详情

Compound 110 (11.17 g, 27.84 mmol) was dried over P2O5 under vacuum at 40° C., then dissolved in dry CH2Cl2 (56 mL, sure seal from Aldrich). 4-dimethylaminopyridine (0.34 g, 2.8 mmol), triethylamine (23.82 mL, 167 mmol) and t-butyldiphenylsilyl chloride were added. The reaction mixture was stirred vigorously for 12 hr. Reaction was monitored by TLC (ethyl acetate:hexane 1:1). It was then diluted with CH2Cl2 (50 mL) and washed with water (3×30 mL) Dichloromethane layer was dried over anhydrous Na2SO4 and evaporated to dryness. Residue purified by flash chromatography (ethyl acetate:hexane 1:1 as eluent) to get 111 as a white foam (8.85 g, 49%). Rf 0.35 (ethyl acetate:hexane, 1:1)

1. customReaction
2. washwashed with water (3×30 mL) Dichloromethane layer
3. dry with materialwas dried over anhydrous Na2SO4
4. customevaporated to dryness
5. customResidue purified by flash chromatography (ethyl acetate:hexane 1:1 as eluent)