Piperazine → 1-(Benzenesulfonyl)piperazine

HRID 914971

반응식

HRID 914971 반응식
[C:1]1([S:7](Cl)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.[NH:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1>C1COCC1>[C:1]1([S:7]([N:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 4837PiperazineHCID 7369Benzenesulfonyl chlorideHCID 8471Triethylamine

생성물 1

HCID 8087121-(Benzenesulfonyl)piperazine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of benzenesulfonyl chloride (1 g, 5.66 mmol) in THF (20 mL) were sequentially added triethylamine (1.97 mL, 14.15 mmol) and piperazine (2.92 g, 33.9 mmol). The reaction was stirred at room temperature for 1 hour before it was extracted with ethyl acetate and washed with water and brine. The ethyl acetate extracts were dried over anhydrous magnesium sulfate and concentrated. The residue was chromatographed on silica gel (1:1 hexanes/ethyl acetate to 10/1 dichloromethane/methanol) to give 22 as a yellow oil.

후처리

  1. extractionwas extracted with ethyl acetate
  2. washwashed with water and brine
  3. dry with materialThe ethyl acetate extracts were dried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was chromatographed on silica gel (1:1 hexanes/ethyl acetate to 10/1 dichloromethane/methanol)

출처 및 근거

ORD 기록
ord-f7a4cdc1ca104faa8100eda6e6bfe630
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07265122B2

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