反应详情

温度

170 °C

6-Methoxy-benzofuran-2,3-dicarboxylic acid diethyl ester (24) (27 g, 92 mmol) is dissolved in 200 ml of a DMSO and the mixture is heated to 170° C. Then sodium chloride (10.7 g, 184 mmol) and water (3.3 ml) are added and the mixture is stirred for 2 h at 160° C. (temperature of reaction mixture). Then the mixture is allowed to cool down and evaporated at high vacuum. The residue is dissolved in ethyl acetate, washed with water and brine and dried over sodium sulfate. Evaporation gave an brown solid, which is further purified by Flash-chromatography (silica gel, ethyl acetate/hexanes 3:7).

1. custom(temperature of reaction mixture)
2. temperatureto cool down
3. customevaporated at high vacuum
4. dissolutionThe residue is dissolved in ethyl acetate
5. washwashed with water and brine
6. dry with materialdried over sodium sulfate
7. customEvaporation
8. customgave an brown solid, which
9. customis further purified by Flash-chromatography (silica gel, ethyl acetate/hexanes 3:7)