反応 #64960

反応方程式

ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

→

2,5-Dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane

溶媒

water

反応条件

後処理

1. 1
   ろ過The BaCO3 is filtered off with suction, K2CO3
2. 2
   workup.ADDITIONis added to the filtrate
3. 3
   ろ過the solid is filtered off with suction again
4. 4
   抽出the filtrate is extracted ten times with 100 ml of CHCl3 each time
5. 5
   乾燥The extracts are dried over K2CO3
6. 6
   濃縮concentrated
7. 7
   workup.DISTILLATIONthe residue is distilled

実験手順

13 g (60.6 mmol) of ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate are heated under reflux with 33 g of Ba(OH)2.8H2O in 330 ml of water overnight. The BaCO3 is filtered off with suction, K2CO3 is added to the filtrate, the solid is filtered off with suction again and the filtrate is extracted ten times with 100 ml of CHCl3 each time. The extracts are dried over K2CO3 and concentrated and the residue is distilled.

出典