反应详情

Alcohol Compound 40 (48.8 g, 0.16 mmol) was added to a mixture of NaH (4.0 g, 0.17 mol) in dry THF (500 mL). After 5 min, MeI (10 mL, 0.17 mol) was added and, after another 3 hours, the mixture was quenched with H2O (150 mL), extracted into diethyl ether (500 mL), dried (MgSO4) and concentrated. Purification of the residue by silica-gel column chromatography [eluent: hexane/ethyl acetate, 90/10, v/v] yielded 1-O-benzyl-3-O-t-butyldimethylsilyl-2-O-methyl-rac-glycerol (Compound 41) (37 g, 74%) as a yellow oil.

1. customthe mixture was quenched with H2O (150 mL)
2. extractionextracted into diethyl ether (500 mL)
3. dry with materialdried (MgSO4)
4. concentrationconcentrated
5. customPurification of the residue by silica-gel column chromatography [eluent: hexane/ethyl acetate, 90/10, v/v]