反应详情

Ethyl chloroformate (0.029 mL) was added to a 0° C. solution of 4-chloro-3-hydroxybenzoic acid (50 mg) and 4-methylmorpholine (0.092 L) in dichloromethane (2 mL). The reaction was stirred for two hours and then was treated with the compound prepared in Example 9 (79 mg). The reaction was stirred overnight, then diluted with ethyl acetate and washed twice with a saturated aqueous sodium bicarbonate solution. The organic phase was dried over anhydrous magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:9, then methanol:concentrated aqueous ammonia:ethyl acetate=2:3:95) to obtain the title compound (60 mg) having the following physical data.

1. stirringThe reaction was stirred overnight
2. washwashed twice with a saturated aqueous sodium bicarbonate solution
3. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
4. concentrationconcentrated
5. customThe residue was purified by column chromatography on silica gel (ethyl acetate