反应详情

温度

160 °C

109 (40 g, 142.7 mmol) is dissolved in 300 ml of a DMSO and after addition of sodium chloride (16.7 g, 285.4 mmol) and water (5.1 ml) the mixture is stirred for 4 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 14.8 g of an red oil, which is further purified by filtration over silica gel (ethyl acetate/hexanes 2:8).

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