HRID36686
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
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
- filtrationThe BaCO3 is filtered off with suction, K2CO3
- additionis added to the filtrate
- filtrationthe solid is filtered off with suction again
- extractionThe filtrate is extracted ten times with 50 ml of CHCl3 each time
- dry with materialthe extracts are dried over K2CO3
- concentrationconcentrated
- distillationthe residue is distilled