HRID1902489

反应详情

EQUATION

反应方程式

HRID 1902489 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.9 g of 4-(3-bromopropionyl)-1,3-dimethyl-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one and 0.75 g of pyrrolidine are warmed at 80° C. for 4 hours in 50 ml of dioxane. After the solvent has been stripped off in vacuo, the residue is taken up in a little saturated sodium carbonate solution. The mixture is extracted three times with 30 ml of ethyl acetate each time, the combined extracts are dried over sodium sulfate, and the solvent is stripped off in vacuo. The remaining crystalline residue is recrystallized from a little acetonitrile. Yield: 1.5 g of the title compound of m.p. 185° C.

WORKUP

后处理

  1. extractionThe mixture is extracted three times with 30 ml of ethyl acetate each time
  2. dry with materialthe combined extracts are dried over sodium sulfate
  3. customThe remaining crystalline residue is recrystallized from a little acetonitrile