HRID1977374
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of ethyl 3-amino-2-[(2′-cyanobiphenyl-4-yl)-methyl]aminobenzoate (5.6 g) and sodium O-ethyl dithiocarbonate (7.3 g) in ethanol (50 ml) was heated for 8 hours under reflux. The reaction mixture was concentrated and the residue was dissolved in water. The solution was adjusted to pH 3-4 with hydrochloric acid. Precipitating crystals were collected by filtration, followed by recrystallization from ethanol to afford yellow crystals (5.0 g, 80%), m.p. 225-227° C.
WORKUP
后处理
- temperaturewas heated for 8 hours
- temperatureunder reflux
- concentrationThe reaction mixture was concentrated
- dissolutionthe residue was dissolved in water
- customPrecipitating crystals
- filtrationwere collected by filtration
- customfollowed by recrystallization from ethanol