HRID2351385

反应详情

EQUATION

反应方程式

HRID 2351385 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.2 g (0.0117 mol) of 11-(chlorocarbonyl)-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one and 1.27 g (0.012 mol) of anhydrous sodium carbonate were heated to 60° C. for 4 hours in 100 ml of dry acetonitrile together with 3.0 g (0.014 mol) of 2-[2-[(diethylamino)-methyl]-piperidin-1-yl]ethanamine with stirring. The mixture was filtered while hot, the filtrate was cooled and the substance which crystallised out was suction filtered. 2.7 g (51% of theory) of colourless cyrstals were obtained, m.p. 175°-176° C.

WORKUP

后处理

  1. filtrationThe mixture was filtered while hot, the filtrate
  2. temperaturewas cooled
  3. customthe substance which crystallised out
  4. filtrationfiltered
  5. custom2.7 g (51% of theory) of colourless cyrstals were obtained