HRID345820

反应详情

EQUATION

反应方程式

HRID 345820 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

9.2 g (42.9 mmol) of ethyl 2,8-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate are heated under reflux with 23.5 g of Ba(OH)2.8H2O in 235 ml of water overnight. The BaCO3 is filtered off with suction, K2CO3 is added to the filtrate and the solid is filtered off with suction again. The filtrate is extracted ten times with 50 ml of CHCl3 each time, the extracts are dried over K2CO3 and concentrated and the residue is distilled.

WORKUP

后处理

  1. filtrationThe BaCO3 is filtered off with suction, K2CO3
  2. additionis added to the filtrate
  3. filtrationthe solid is filtered off with suction again
  4. extractionThe filtrate is extracted ten times with 50 ml of CHCl3 each time
  5. dry with materialthe extracts are dried over K2CO3
  6. concentrationconcentrated
  7. distillationthe residue is distilled