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4-Chlorobenzenesulfonyl chloride → 1H-1,4-Diazepine, 1-[(4-chlorophenyl)sulfonyl]hexahydro-

HRID 2289537
ノート
印刷プレビュー

反応式

HRID 2289537 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[NH:12]1[CH2:18][CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>ClCCl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:12]2[CH2:18][CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)(=[O:10])=[O:9])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 73984-Chlorobenzenesulfonyl chlorideHCID 68163Hexahydro-1,4-diazepine

生成物 1

HCID 116087901H-1,4-Diazepine, 1-[(4-chlorophenyl)sulfonyl]hexahydro-収率 76.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

The 1-(4-chlorophenylsulphonyl)homopiperazine was prepared as follows. 4-Chlorophenylsulphonyl chloride (3.74 g) in dichloromethane (100 ml) was added slowly to a solution of homopiperazine (6.73 g) in dichloromethane (100 ml). The reaction was stood at room temperature overnight. The reaction was washed with water, dried (MgSO4) and the solvent removed in vacuo. The residue was triturated with 20% ether in hexane to give 1-(4-chlorophenylsulphonyl)homopiperazine (3.71 g); NMR (DMSOd6): 1.65 (m, 2H), 2.73 (m, 4H), 3.2-3.65 (m 4H), 7.7 (m, 2H), 7.8 (m, 2H).

後処理

  1. customThe 1-(4-chlorophenylsulphonyl)homopiperazine was prepared
  2. washThe reaction was washed with water
  3. dry with materialdried (MgSO4)
  4. customthe solvent removed in vacuo
  5. customThe residue was triturated with 20% ether in hexane

出典と根拠

ORDレコード
ord-1286599c27e44beaa45237ffe2c7afa0
出典データセット
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06093718

反応ノート

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