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

HRID 916451

반응식

HRID 916451 반응식
[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]

참가 물질

5

반응물 3

HCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 473962983502-55-0

생성물 1

HCID 132894881-Acetyl-4-(2-chloroethyl)piperazine수율 54.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-2f4d03f2efd1421885b5b5b054254a73
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07268230B2

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