反应详情

温度

60 °C

A mixture of acetic anhydride (0.33 mL, 3.57 mmol) and formic acid (0.17 mL, 4.46 mmol) was heated at 60° C. for 2 hours. The reaction mixture was cooled to 0° C., a solution of (4-amino-phenyl)-acetic acid ethyl ester (Preparation 267, 500 mg, 2.79 mmol) in THF (10 mL) was added slowly to the reaction mixture and the reaction was allowed to stir at room temperature for 16 hours. The reaction mixture was neutralized with sat. aq. Na2CO3 solution and extracted with diethyl ether (2×25 mL). The combined organic layers were dried (Na2SO4) and evaporated in vacuo. The crude material was purified by column chromatography on silica gel (gradient of DCM:MeOH 100:0 to 98:2) to afford the title compound as an oil in 93% yield, 500 mg.

1. temperatureThe reaction mixture was cooled to 0° C.
2. extractionextracted with diethyl ether (2×25 mL)
3. dry with materialThe combined organic layers were dried (Na2SO4)
4. customevaporated in vacuo
5. customThe crude material was purified by column chromatography on silica gel (gradient of DCM:MeOH 100:0 to 98:2)