p-Bromobenzenesulfonyl chloride → 1-(4-Bromophenylsulfonyl)-4-methylpiperazine

HRID 17954

반응식

HRID 17954 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.C(=O)(O)[O-].[Na+].[CH3:17][N:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1>ClCCl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:21]2[CH2:22][CH2:23][N:18]([CH3:17])[CH2:19][CH2:20]2)(=[O:10])=[O:9])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 7396p-Bromobenzenesulfonyl chlorideHCID 531671-MethylpiperazineHCID 516892Sodium Bicarbonate

생성물 1

HCID 7107291-(4-Bromophenylsulfonyl)-4-methylpiperazine

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 4-bromobenzene-1-sulfonyl chloride (256 mg, 1.00 mmol) in 1 mL of dichloromethane was slowly added to a vial (40 mL) containing 5 mL of a saturated aqueous solution of sodium bicarbonate, dichloromethane (5 mL) and 1-methylpiperazine (100 mg, 1.00 mmol). The reaction was stirred at room temperature overnight. The phases were separated and the organic layer was dried over magnesium sulfate. Evaporation of the solvent under reduced pressure provided the required product, which was used in the next step without further purification. ESI-MS m/z calc. 318.0. found 318.9 (M+1)+. Retention time of 1.30 minutes. 1H NMR (300 MHz, CDCl3) δ 7.65 (d, J=8.7 Hz, 2H), 7.58 (d, J=8.7 Hz, 2H), 3.03 (t, J=4.2 Hz, 4H), 2.48 (t, J=4.2 Hz, 4H), 2.26 (s, 3H).

후처리

  1. customThe phases were separated
  2. dry with materialthe organic layer was dried over magnesium sulfate
  3. customEvaporation of the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-98148ec2c0304d52aa28b7f15b9bb935
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741321B2

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