反应详情

In 20 ml of chlorobenzene were dissolved 1.1 g (5.0 mmol) of 4-phenyl-1,2,3-thiadiazole-5-carbothioamide and 0.92 g (5.0 mmol) of methyl bromopyruvate. The solution thus obtained was stirred for 3 hours with heating under reflux. After the reaction was completed, the reaction mixture was cooled to room temperature, a saturated aqueous solution of sodium hydrogen carbonate was added thereto, and the objective product was extracted with ethyl acetate. The solvent was distilled off from the extract solution under a reduced pressure, and the residue was purified by silica gel column chromatography using 3:1 mixture of n-hexane and ethyl acetate. Thus, 0.74 g of the objective compound was obtained.

1. customThe solution thus obtained
2. temperaturewith heating
3. temperatureunder reflux
4. extractionthe objective product was extracted with ethyl acetate
5. distillationThe solvent was distilled off from the extract solution under a reduced pressure
6. customthe residue was purified by silica gel column chromatography
7. addition3:1 mixture of n-hexane and ethyl acetate