Triethylamine → 1-[4-(1-Acetimidoylpiperidin-4-yl)benzoyl]-4-(6-chloronaphthalene-2-sulfonyl)piperazine hydrochloride

HRID 278608ノート

反応式

HRID 278608 の反応式
Cl.[NH:2]1[CH2:7][CH2:6][CH:5]([C:8]2[CH:35]=[CH:34][C:11]([C:12]([N:14]3[CH2:19][CH2:18][N:17]([S:20]([C:23]4[CH:32]=[CH:31][C:30]5[C:25](=[CH:26][CH:27]=[C:28]([Cl:33])[CH:29]=5)[CH:24]=4)(=[O:22])=[O:21])[CH2:16][CH2:15]3)=[O:13])=[CH:10][CH:9]=2)[CH2:4][CH2:3]1.[CH2:36]([N:38](CC)CC)[CH3:37].Cl.C(=N)(OCC)C>CO>[ClH:33].[C:36]([N:2]1[CH2:7][CH2:6][CH:5]([C:8]2[CH:35]=[CH:34][C:11]([C:12]([N:14]3[CH2:19][CH2:18][N:17]([S:20]([C:23]4[CH:32]=[CH:31][C:30]5[C:25](=[CH:26][CH:27]=[C:28]([Cl:33])[CH:29]=5)[CH:24]=4)(=[O:22])=[O:21])[CH2:16][CH2:15]3)=[O:13])=[CH:10][CH:9]=2)[CH2:4][CH2:3]1)(=[NH:38])[CH3:37]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 2724290Ethanimidic acid, ethyl ester, hydrochloride (1:1)HCID 227110601-(6-Chloronaphthalene-2-sulfonyl)-4-[4-(4-piperidyl)benzoyl]piperazine hydrochloride

生成物 1

HCID 226280911-[4-(1-Acetimidoylpiperidin-4-yl)benzoyl]-4-(6-chloronaphthalene-2-sulfonyl)piperazine hydrochloride収率 195%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 1-[4-(piperidin-4-yl)benzoyl]-4-(6-chloronaphthalene-2-sulfonyl)piperazine hydrochloride (40 mg) and triethylamine (156 mg) in methanol (15 ml) was added ethyl acetimidate hydrochloride (46 mg), and the solution was stirred at room temperature for 15 hours. The reaction solution was concentrated. To the residue was added 1 N sodium hydroxide solution, and the solution was extracted with dichloromethane. The extract was dried and concentrated. The residue was dissolved in ethyl acetate, to which was added 4 N hydrochloric acid in ethyl acetate. The precipitate was filtered, washed with ether and dried to give a colorless solid of the title compound (42 mg).

後処理

  1. concentrationThe reaction solution was concentrated
  2. additionTo the residue was added 1 N sodium hydroxide solution
  3. extractionthe solution was extracted with dichloromethane
  4. customThe extract was dried
  5. concentrationconcentrated
  6. dissolutionThe residue was dissolved in ethyl acetate, to which
  7. additionwas added 4 N hydrochloric acid in ethyl acetate
  8. filtrationThe precipitate was filtered
  9. washwashed with ether
  10. customdried

出典と根拠

ORDレコード
ord-13a54221185a48bfbe3cbef54115fb73
出典データセット
uspto-grants-2002_03
特許番号
US06359134B1

反応ノート

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