Triethylamine → HCID 178479693、化合物

HRID 278620

反応式

HRID 278620 の反応式
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

参加物

5

反応物 3

HCID 8471TriethylamineHCID 883692-Methylthio-2-imidazoline hydroiodideHCID 178479260HCID 178479260、化合物

生成物 1

HCID 178479693HCID 178479693、化合物収率 52.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-0b9c4a1b28694e43996b770efe9ae48b
出典データセット
uspto-grants-2002_03
特許番号
US06359134B1

関連ノート

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