反应详情

温度

40 °C

6.1 ml of 2M sodium hydroxide solution are added dropwise to a mixture of 1.6 g of 6,6,7-trifluoro-6,7-dihydro-1H-[1,4]-dioxino[2,3-f]benzimidazole-2-thiol and 1.4 g of 2-chloromethyl-4-methoxy-3,5-dimethylpyridine hydrochloride in 40 ml of ethanol at room temperature and the mixture is stirred at 40° C. for 5 h. The solvent is distilled off in vacuo, water is added, the mixture is extracted with methylene chloride, the organic solution is concentrated and the residue is recrystallized from ethanol and water. 1.9 g (77%) of the title compound of m.p. 138°-140° C. are obtained.

1. distillationThe solvent is distilled off in vacuo, water
2. additionis added
3. extractionthe mixture is extracted with methylene chloride
4. concentrationthe organic solution is concentrated
5. customthe residue is recrystallized from ethanol and water