Water → 1-(4-Bromophenyl)-4-(methylsulfonyl)piperazine

HRID 40694

反応式

HRID 40694 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH3:21][S:22](Cl)(=[O:24])=[O:23].O>ClCCl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([S:22]([CH3:21])(=[O:24])=[O:23])[CH2:10][CH2:9]2)=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 27356291-(4-Bromophenyl)piperazine

生成物 1

HCID 219193841-(4-Bromophenyl)-4-(methylsulfonyl)piperazine収率 99.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1-(4-Bromophenyl)piperazine (5 g, 20.7 mmol) is placed in 104 ml of dichloromethane and then triethylamine (4.34 ml, 31.1 mmol) is added, followed, dropwise, by methanesulfonyl chloride (1.93 ml, 24.9 mmol). Stirring is maintained for 16 h. After the addition of 30 ml of water and stirring, the organic phase is washed with a saturated aqueous sodium chloride solution, dried over MgSO4 and concentrated. 6.6 g of expected 1-(4-bromophenyl)-4-methanesulfonylpiperazine are obtained.

後処理

  1. temperatureis maintained for 16 h
  2. stirringstirring
  3. washthe organic phase is washed with a saturated aqueous sodium chloride solution
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-bb724b676d6c4ddc89c7c0ee5d97c752
出典データセット
uspto-grants-2013_09
特許番号
US08530477B2

関連ノート

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