Triethylamine → HCID 178479693, 화합물

HRID 278620

반응식

HRID 278620 반응식
Cl.[NH2:2][C@H:3]1[CH2:8][CH2:7][C@H:6]([C:9]([N:11]2[CH2:16][CH2:15][N:14]([S:17]([C:20]3[CH:29]=[CH:28][C:27]4[C:22](=[CH:23][CH:24]=[C:25]([Cl:30])[CH:26]=4)[CH:21]=3)(=[O:19])=[O:18])[CH2:13][CH2:12]2)=[O:10])[CH2:5][CH2:4]1.C(N(CC)CC)C.CS[C:40]1[NH:41][CH2:42][CH2:43][N:44]=1>C(O)C>[ClH:30].[Cl:30][C:25]1[CH:26]=[C:27]2[C:22](=[CH:23][CH:24]=1)[CH:21]=[C:20]([S:17]([N:14]1[CH2:13][CH2:12][N:11]([C:9]([C@H:6]3[CH2:7][CH2:8][C@H:3]([NH:2][N:44]4[CH2:43][CH2:42][N:41]=[CH:40]4)[CH2:4][CH2:5]3)=[O:10])[CH2:16][CH2:15]1)(=[O:18])=[O:19])[CH:29]=[CH:28]2

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 883692-Methylthio-2-imidazoline hydroiodideHCID 178479260HCID 178479260, 화합물

생성물 1

HCID 178479693HCID 178479693, 화합물수율 52.4%

시약·촉매·용매 1

HCID 702Ethanol용매

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).

후처리

  1. temperaturethe mixture was heated for 48 hours
  2. temperatureunder reflux
  3. concentrationThe reaction solution was concentrated
  4. customthe residue was purified with silica gel column chromatography (dichloromethane/methanol containing 10% ammonia=10/1)

출처 및 근거

ORD 기록
ord-0b9c4a1b28694e43996b770efe9ae48b
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06359134B1

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