反应详情

0.6 ml of 3-chloromethylbenzoyl chloride is added dropwise, at 0° C., to 1.6 g of the compound of Example 4 dissolved in 10 ml of anhydrous pyridine. After 2 hours at 0° C., methanol is added to hydrolyze the excess acid chloride and the organic phase is diluted with methylene chloride. This is then washed with 2N hydrochloric acid, with saturated aqueous sodium bicarbonate and then with saturated aqueous sodium chloride and dried over anhydrous sodium sulphate. The organic solvent is evaporated off and the product is purified on a column of silica, using a mixture of cyclohexane and ethyl acetate (20:1 v/v) as eluent, to give the expected product.

1. washThis is then washed with 2N hydrochloric acid, with saturated aqueous sodium bicarbonate
2. dry with materialwith saturated aqueous sodium chloride and dried over anhydrous sodium sulphate
3. customThe organic solvent is evaporated off
4. customthe product is purified on a column of silica
5. additiona mixture of cyclohexane and ethyl acetate (20:1 v/v) as eluent