反应详情

A mixture of methyl 2-hydroxy-6-methylbenzoate (prepared according to Doehner et al, WO 01/05739, 10.0 g), tert-butyldimethylsilyl chloride (11.0 g), N,N-di-isopropylethylamine (32 mL) and DMAP (0.75 g) in DCM (400 mL) was stirred at room temperature overnight. The mixture was washed with water and brine, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was purified by chromatography on silica eluting with a mixture of ethyl acetate and pentane with a gradient of 0-10% to give methyl 2-(tert-butyldimethylsilyloxy)-6-methylbenzoate (11.9 g) as an oil.

1. washThe mixture was washed with water and brine
2. dry with materialdried (MgSO4)
3. filtrationfiltered
4. customThe filtrate was evaporated to dryness
5. customthe residue was purified by chromatography on silica eluting with a mixture of ethyl acetate and pentane with a gradient of 0-10%