반응 #305510

반응 방정식

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

용매

1,2-dichloroethane

반응 조건

후처리

1. 1
   농축The reaction mixture was concentrated in vacuo
2. 2
   기타After 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
   온도under reflux for one hour
6. 6
   농축the reaction mixture was concentrated in vacuo
7. 7
   기타The resulting 2-(5-phenyl-[1,2,4]oxadiazol-3-yl)-morpholine hydrochloride (intermediate 28) was used for next reaction without further purification

실험 절차

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.

출처