반응 #64969

반응 방정식

ethyl 2-(tetrahydropyran-2-yl)-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

perchloric acid

sodium methylate

→

Ethyl 3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

용매

ethanol

반응 조건

후처리

1. 1
   농축the mixture is concentrated
2. 2
   추출extracted with CHCl3
3. 3
   건조The extract is dried over K2CO3
4. 4
   농축concentrated
5. 5
   workup.DISTILLATIONthe residue is distilled

실험 절차

15 g (55.5 mmol) of ethyl 2-(tetrahydropyran-2-yl)-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate are heated under reflux with 8.25 g (56 mmol) of 70% strength perchloric acid in 100 ml of ethanol for 30 minutes. 10.5 g (58 mmol) of 30 strength sodium methylate solution are added, the mixture is concentrated, the residue is taken up in water and the solution is saturated with K2CO3 and extracted with CHCl3. The extract is dried over K2CO3 and concentrated and the residue is distilled.

출처