반응 #305506

반응 방정식

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

용매

1,2-dichloroethane

반응 조건

후처리

1. 1
   기타4 hours
2. 2
   농축The reaction mixture was concentrated in vacuo
3. 3
   기타After 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
   온도under reflux
7. 7
   농축the reaction mixture was concentrated in vacuo
8. 8
   기타The resulting 2-(3-phenyl-[1,2,4]oxadiazol-5-yl)-morpholine hydrochloride (intermediate 22) was used for next reaction without further purification

실험 절차

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.

출처