HRID1645979
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe aqueous phase is separated off
- extractionextracted twice with 100 ml of methylene chloride each time
- dry with materialThe organic solutions are dried over magnesium sulphate
- concentrationconcentrated
- distillationthe residue is distilled