反应详情

温度

180 °C

To a solution of the product of Example 2 (65 g) in dimethyl sulfoxide (65 g) is added sodium chloride (1 g). The mixture is stirred while warming at about 180° C., and water is added in small portions while maintaining the temperature between 170° and 180°. Ethanol and water are evolved and are removed by distillation until about 60 ml of liquid has been collected. The mixture is cooled, ether (200 ml) added, and the mixture partitioned with 3 portions of water (50 ml). The organic phase is dried over sodium sulfate and evaporated to a residue. Distillation of the residue gives the title product (25 g) (57%) B.P. 38° (0.01 mm) nD26 1.4400.

1. temperaturewhile maintaining the temperature between 170° and 180°
2. customare removed by distillation until about 60 ml of liquid
3. customhas been collected
4. temperatureThe mixture is cooled
5. additionether (200 ml) added
6. customthe mixture partitioned with 3 portions of water (50 ml)
7. dry with materialThe organic phase is dried over sodium sulfate
8. customevaporated to a residue
9. distillationDistillation of the residue