반응 #365802

ord-0b9c4a1b28694e43996b770efe9ae48b

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture was heated for 48 hours
  2. 2
    온도under reflux
  3. 3
    농축The reaction solution was concentrated
  4. 4
    기타the 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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06359134B1uspto-grants-2002_03