HRID1263407

反应详情

EQUATION

反应方程式

HRID 1263407 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction mixture was heated at 90° C. for 3 h
  2. filtrationthe precipitate was filtered off with suction
  3. washwashed with methylene chloride
  4. dissolutionThe precipitate was then dissolved in ethyl acetate
  5. extractionextracted with sodium bicarbonate solution
  6. washAfter washing
  7. customdrying
  8. customthe product was obtained