Reaktion #305510

Reaktionsgleichung

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

intermediate 27

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

chloroethyl chloroformate

→

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

Lösungsmittel

1,2-dichloroethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe reaction mixture was concentrated in vacuo
2. 2
   SonstigeAfter removal of the solvent
3. 3
   workup.DISSOLUTIONthe residue was dissolved in methanol (2.0 ml)
4. 4
   workup.STIRRINGthe solution was stirred
5. 5
   Temperaturunder reflux for one hour
6. 6
   Einengenthe reaction mixture was concentrated in vacuo
7. 7
   SonstigeThe resulting 2-(5-phenyl-[1,2,4]oxadiazol-3-yl)-morpholine hydrochloride (intermediate 28) was used for next reaction without further purification

Vorschrift

To a stirred solution of 4-benzyl-2-(5-phenyl-1,2,4-oxadiazol-3-yl)morpholine (intermediate 27, 900 mg, 2.80 mmol) in 1,2-dichloroethane (2.0 ml) was added chloroethyl chloroformate (0.46 ml, 4.20 mmol), and the reaction mixture was stirred at 70° C. for 4 hours. The reaction mixture was concentrated in vacuo. After removal of the solvent, the residue was dissolved in methanol (2.0 ml), and the solution was stirred under reflux for one hour. When the reaction was complete (checked by thin layer chromatography), the reaction mixture was concentrated in vacuo. The resulting 2-(5-phenyl-[1,2,4]oxadiazol-3-yl)-morpholine hydrochloride (intermediate 28) was used for next reaction without further purification.

Quelle