HRID356176
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 solution of (3aR*,10aS*)-9-benzyl-4-(chloroacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]-cyclopenta[e][1,4]diazepin-10(1H)-one (1.0 g, 2.7 mmol) and dibenzylamine (5.36 g, 27.1 mmol) in 1,2-dichloroethane (30 mL) was refluxed for 17 hours, to which was added a saturated aqueous solution of sodium hydrogencarbonate, followed by extraction with dichloromethane. The extract solution was washed with water and dried, followed by distilling off the solvent. The residue was purified by silica-gel column chromatography (ethyl acetate-hexane 1:1) to give 0.40 g (yield 28%) as an oily product.
WORKUP
后处理
- extractionfollowed by extraction with dichloromethane
- washThe extract solution was washed with water
- customdried
- distillationby distilling off the solvent
- customThe residue was purified by silica-gel column chromatography (ethyl acetate-hexane 1:1)
- customto give 0.40 g (yield 28%) as an oily product