Reaktion #64960

Reaktionsgleichung

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

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe BaCO3 is filtered off with suction, K2CO3
2. 2
   workup.ADDITIONis added to the filtrate
3. 3
   Filtrationthe solid is filtered off with suction again
4. 4
   Extraktionthe filtrate is extracted ten times with 100 ml of CHCl3 each time
5. 5
   TrocknenThe extracts are dried over K2CO3
6. 6
   Einengenconcentrated
7. 7
   workup.DISTILLATIONthe residue is distilled

Vorschrift

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.

Quelle