HRID1645979

反应详情

EQUATION

反应方程式

HRID 1645979 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

13 g (61.2 mmol) of tert.-butyl 2,7-diazabicyclo[3.3.0]octane-7-carboxylate are dissolved in 100 ml of toluene, a solution of 3 g of sodium hydroxide in 20 ml of water is added and 7 g (64.5 mmol) of ethyl chloroformate are added dropwise at room temperature. The mixture is stirred for three hours at room temperature, and the aqueous phase is separated off and extracted twice with 100 ml of methylene chloride each time. The organic solutions are dried over magnesium sulphate and concentrated, and the residue is distilled.

WORKUP

后处理

  1. customthe aqueous phase is separated off
  2. extractionextracted twice with 100 ml of methylene chloride each time
  3. dry with materialThe organic solutions are dried over magnesium sulphate
  4. concentrationconcentrated
  5. distillationthe residue is distilled