反应详情

A mixture of ethyl 3-bromo-6-bromomethyl-2-methoxybenzoate (Intermediate 87, 0.262 g), 2-methylthiophenol (0.096 ml) and potassium carbonate (0.28 g) in THF (5 ml) was stirred at room temperature for 3 days. The resultant mixture was partitioned between ethyl acetate and NaHCO3 (saturated aqueous solution). The separated organic phase was 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 cyclohexane with a gradient of 0-30% to give ethyl 3-bromo-2-methoxy-(2-methylphenylthiomethyl)benzoate (0.24 g) as a gum.

1. customThe resultant mixture was partitioned between ethyl acetate and NaHCO3 (saturated aqueous solution)
2. dry with materialThe separated organic phase was dried (MgSO4)
3. filtrationfiltered
4. customThe filtrate was evaporated to dryness
5. customthe residue was purified by chromatography on silica
6. washeluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-30%