反应详情

温度

100 °C

A mixture of 4-chloro-2-nitrobenzoic acid methyl ester 100 mg, prolinol 235 mg and 1-methyl-2-pyrrolidinone 3 ml is stirred at 100° C. for 3 hours. After cooling to room temperature, ethyl acetate and water are added to the mixture. The organic layer is washed with water (twice) and brine, and dried over sodium sulfate. After removal of the sodium sulfate, the filtrate is concentrated in vacuo, and the residue is purified with preparative thin-layer chromatography (two plates, solvent; hexane:ethyl acetate=1:1) to give 4-(2-hydroxymethyl-1-pyrrolidinyl)-2-nitrobenzoic acid methyl ester 20 mg as a yellow oil. MS(m/z): 281 (M+H)+

1. temperatureAfter cooling to room temperature
2. washThe organic layer is washed with water (twice) and brine
3. dry with materialdried over sodium sulfate
4. customAfter removal of the sodium sulfate
5. concentrationthe filtrate is concentrated in vacuo
6. customthe residue is purified with preparative thin-layer chromatography (two plates, solvent; hexane:ethyl acetate=1:1)