반응 #44398

ord-6738cef98f8145c9991bc3321e90ddd0

반응 방정식

Cl.Cl.Cl.N[C@H]1CC[C@H](CCN2CCN(c3cccc(Cl)c3Cl)CC2)CC1
trans-4-{2-[4-(2,3-dichlorophenyl)-piperazin-1-yl]-ethyl}-cyclohexyl-amine trihydrochloride
CCN(CC)CC
triethylamine
CN(C)C(=O)Cl
N,N-dimethylcarbamoylchloride
CN(C)C(=O)N[C@H]1CC[C@H](CCN2CCN(c3cccc(Cl)c3Cl)CC2)CC1
title compound
수율 65.0%
CN(C)C(=O)N[C@H]1CC[C@H](CCN2CCN(c3cccc(Cl)c3Cl)CC2)CC1
Trans-1-{4-[2-[4-(2,3-dichlorophenyl)-piperazin-1-yl]-ethyl]-cyclohexyl}-3,3-dimethyl-urea
수율 65.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과filtered
  2. 2
    세척The filtrate was washed with water (2×20 ml)
  3. 3
    기타dried
  4. 4
    기타evaporated in vacuo
  5. 5
    기타Recrystallizing from methanol

실험 절차

1.39 g (3 mmol) trans-4-{2-[4-(2,3-dichlorophenyl)-piperazin-1-yl]-ethyl}-cyclohexyl-amine trihydrochloride was suspended in dichloromethane (100 ml), triethylamine (2.1 ml, 15 mmol) was added followed by 0.30 ml (3.3 mmol) N,N-dimethylcarbamoylchloride. The reaction mixture was stirred for 48 hours at room temperature, filtered. The filtrate was washed with water (2×20 ml), dried and evaporated in vacuo. Recrystallizing from methanol gave the title compound (0.83 g, 65%), melting at 212-4° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07737142B2uspto-grants-2010_06