반응 #64964

반응 방정식

ethyl 2,8-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

→

2,8-Dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane

용매

water

반응 조건

후처리

1. 1
   여과The BaCO3 is filtered off with suction, K2CO3
2. 2
   workup.ADDITIONis added to the filtrate
3. 3
   여과the solid is filtered off with suction again
4. 4
   추출The filtrate is extracted ten times with 50 ml of CHCl3 each time
5. 5
   건조the extracts are dried over K2CO3
6. 6
   농축concentrated
7. 7
   workup.DISTILLATIONthe residue is distilled

실험 절차

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.

출처