반응 #590159

반응 방정식

7-Methoxy-3,4,5,6-tetrahydro-2H-azepine

dioxane

1-(3-chloro-4-methyl-2-thienyl)cyclopentane-carbohydrazide

→

3-[1-(3-chloro-4-methyl-2-thienyl)cyclopentyl]-6,7,8,9-tetrahydro-5H-[1,2,4]triazolo[4,3-a]azepine

용매

toluene

반응 조건

후처리

1. 1
   기타The reaction solution was subjected to evaporation under reduced pressure
2. 2
   기타the resulting crude product was purified by column chromatography (chloroform:methanol=40:1)
3. 3
   세척The resulting solid was washed with hexane

실험 절차

7-Methoxy-3,4,5,6-tetrahydro-2H-azepine (0.5 ml) was added to a dioxane (20 ml) and toluene (15 ml) solution of 1-(3-chloro-4-methyl-2-thienyl)cyclopentane-carbohydrazide (800 mg), followed by stirring at 100° C. for 3 days. The reaction solution was subjected to evaporation under reduced pressure and the resulting crude product was purified by column chromatography (chloroform:methanol=40:1). The resulting solid was washed with hexane to obtain 770 mg of 3-[1-(3-chloro-4-methyl-2-thienyl)cyclopentyl]-6,7,8,9-tetrahydro-5H-[1,2,4]triazolo[4,3-a]azepine (colorless solid).

출처