HRID356176

反应详情

EQUATION

反应方程式

HRID 356176 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionfollowed by extraction with dichloromethane
  2. washThe extract solution was washed with water
  3. customdried
  4. distillationby distilling off the solvent
  5. customThe residue was purified by silica-gel column chromatography (ethyl acetate-hexane 1:1)
  6. customto give 0.40 g (yield 28%) as an oily product