反应详情

A mixture of 115 mg of 5-[2-(2,5-dimethoxyphenyl)ethyl]-2-amino benzoic acid methylester and 50 mg of 4-dimethylaminopyridine in 6 ml of dry dichloromethane is treated with 35 mg of methyl chloroformiate and stirred for 3 hours at room temperature. Then the mixture is poured onto aqueous pH7 buffer solution and extracted with ethyl acetate. The combined organic extracts are dried over magnesium sulfate and concentrated in vacuo. The crude product is purified by silica gel chromatography (cyclohexane/ethyl acetate=8/1) to yield the title compound as colourless crystals. mp: 80-82°.

1. additionis treated with 35 mg of methyl chloroformiate
2. extractionextracted with ethyl acetate
3. dry with materialThe combined organic extracts are dried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe crude product is purified by silica gel chromatography (cyclohexane/ethyl acetate=8/1)