반응 #365802
ord-0b9c4a1b28694e43996b770efe9ae48b
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상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도the mixture was heated for 48 hours
- 2온도under reflux
- 3농축The reaction solution was concentrated
- 4기타the residue was purified with silica gel column chromatography (dichloromethane/methanol containing 10% ammonia=10/1)
실험 절차
To a solution of 1-(trans-4-aminocyclohexane-1-ylcarbonyl)-4-(6-chloronaphthalene-2-sulfonyl)piperazine hydrochloride (100 mg) and triethylamine (120 mg) in ethanol (10 ml) was added 2-methylthioimidazoline (116 mg), and the mixture was heated for 48 hours under reflux. The reaction solution was concentrated, and the residue was purified with silica gel column chromatography (dichloromethane/methanol containing 10% ammonia=10/1) and transformed into hydrochloride with 4 N hydrochloric acid in ethyl acetate to give a colorless solid of the title compound (30 mg).