4-Toluenesulfonyl chloride → 1-Acetyl-4-(2-chloroethyl)piperazine

HRID 916451

反応式

HRID 916451 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][N:7]([CH2:10][CH2:11]O)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].C(N(CC)CC)C.C1(C)C=CC(S([Cl:29])(=O)=O)=CC=1>C(Cl)Cl>[C:1]([N:4]1[CH2:9][CH2:8][N:7]([CH2:10][CH2:11][Cl:29])[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 47396291-Acetyl-4-(2-hydroxyethyl)piperazine

生成物 1

HCID 132894881-Acetyl-4-(2-chloroethyl)piperazine収率 54.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2-(4-Acetylpiperazin-1-yl)ethanol (500 mg, 2.90 mmol), (prepared as described for the starting material in this example hereinbefore), was dissolved in methylene chloride (10 ml) and triethylamine (445 μl, 3.19 mmol) and 4-toluenesulphonyl chloride (609 mg, 3.19 mmol) were added and the mixture was stirred at ambient temperature overnight. The mixture was washed with brine, dried (MgSO4) and concentrated under reduced pressure. The residue was purified by column chromatography eluting with methylene chloride/methanol (98/2) to give 1-acetyl-4-(2-chloroethyl)piperazine (300 mg, 54%) as an oil.

後処理

  1. washThe mixture was washed with brine
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by column chromatography
  5. washeluting with methylene chloride/methanol (98/2)

出典と根拠

ORDレコード
ord-2f4d03f2efd1421885b5b5b054254a73
出典データセット
uspto-grants-2007_09
特許番号
US07268230B2

関連ノート

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