HRID1263407
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
56 g of N-(2-methyl-3-methoxycarbonylphenyl)thiourea (0.25 mol) were dissolved in 2 l of chlorobenzene, and the mixture was cooled to 0° C. 40 g of bromine (0.25 mol) in 100 ml of chlorobenzene were then added dropwise. The reaction mixture was heated at 90° C. for 3 h, and the precipitate was filtered off with suction and washed with methylene chloride. The precipitate was then dissolved in ethyl acetate and extracted with sodium bicarbonate solution. After washing and drying, the product was obtained by stripping off the solvent. Yield: 43 g (80%).
WORKUP
后处理
- temperatureThe reaction mixture was heated at 90° C. for 3 h
- filtrationthe precipitate was filtered off with suction
- washwashed with methylene chloride
- dissolutionThe precipitate was then dissolved in ethyl acetate
- extractionextracted with sodium bicarbonate solution
- washAfter washing
- customdrying
- customthe product was obtained