HRID1701303

反应详情

EQUATION

反应方程式

HRID 1701303 的结构方程式

PROCEDURE

实验过程

130 g. of o-phenylenediamine, 121 g. of 5-ethyl-2-methylpyridine and 96 g. of sulfur were heated at 160°-170° C. for 20 hours. The reaction mixture was dissolved in 2,000 ml. of chloroform and the solution was washed with water and 6 N hydrochloric acid successively. Chloroform was removed by evaporation in vacuo. The residue was subjected to silica gel column chromatography and recrystallized from ethyl acetate. The product showed no melting point depression upon mixing with the product of the preceding example. Yield, 137 g (61% of theory).

WORKUP

后处理

  1. dissolutionThe reaction mixture was dissolved in 2,000 ml
  2. washof chloroform and the solution was washed with water and 6 N hydrochloric acid successively
  3. customChloroform was removed by evaporation in vacuo
  4. customrecrystallized from ethyl acetate
  5. customYield