HRID1701303
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- dissolutionThe reaction mixture was dissolved in 2,000 ml
- washof chloroform and the solution was washed with water and 6 N hydrochloric acid successively
- customChloroform was removed by evaporation in vacuo
- customrecrystallized from ethyl acetate
- customYield