Reaktion #305506

Reaktionsgleichung

4-benzyl-2-(3-phenyl-1,2,4-oxadiazol-5-yl)morpholine

intermediate 21

4-benzyl-2-(3-phenyl-1,2,4-oxadiazol-5-yl)morpholine

chloroethyl chloroformate

→

2-(3-Phenyl-[1,2,4]oxadiazol-5-yl)-morpholine Hydrochloride

Lösungsmittel

1,2-dichloroethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstige4 hours
2. 2
   EinengenThe reaction mixture was concentrated in vacuo
3. 3
   SonstigeAfter removal of the solvent
4. 4
   workup.DISSOLUTIONthe residue was dissolved in methanol (10 ml)
5. 5
   workup.STIRRINGthe reaction solution was stirred for one hour
6. 6
   Temperaturunder reflux
7. 7
   Einengenthe reaction mixture was concentrated in vacuo
8. 8
   SonstigeThe resulting 2-(3-phenyl-[1,2,4]oxadiazol-5-yl)-morpholine hydrochloride (intermediate 22) was used for next reaction without further purification

Vorschrift

To a stirred solution of 4-benzyl-2-(3-phenyl-1,2,4-oxadiazol-5-yl)morpholine (intermediate 21, 2.0 g, 6.22 mmol) in 1,2-dichloroethane (10 ml) was added chloroethyl chloroformate (2.0 ml, 18.7 mmol), and the reaction mixture was stirred for at 70° C. 4 hours. The reaction mixture was concentrated in vacuo. After removal of the solvent, the residue was dissolved in methanol (10 ml), and the reaction solution was stirred for one hour under reflux. When the reaction was complete (checked by thin layer chromatography), the reaction mixture was concentrated in vacuo. The resulting 2-(3-phenyl-[1,2,4]oxadiazol-5-yl)-morpholine hydrochloride (intermediate 22) was used for next reaction without further purification.

Quelle