HRID355908
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 0.291 g of 6,11-dihydro-5H-di-benz[b,e]azepine, 0.518 g of 4-[N-methyl-N-(2-methyl-benzoyl)amino]benzoyl chloride and 0.182 g of triethylamine in 10 ml of tetrahydrofuran is stirred at room temperature for 2 hours. The solyent is removed, the residue diluted with water and extracted with dichloromethane. The extract is washed with 1 N HCl water, 1M NaHCO3, brine and dried (Na2SO4). The solution is passed through a thin pad of hydrous magnesium silicate. The filtrate is concentrated and chilled to give 0.52 g of crystals, m.p. 160°-170° C.
WORKUP
后处理
- customThe solyent is removed
- additionthe residue diluted with water
- extractionextracted with dichloromethane
- washThe extract is washed with 1 N HCl water, 1M NaHCO3, brine
- dry with materialdried (Na2SO4)
- concentrationThe filtrate is concentrated
- temperaturechilled