Piperazine → 1-(Benzenesulfonyl)piperazine

HRID 914971

反応式

HRID 914971 の反応式
[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

参加物

5

反応物 3

HCID 4837PiperazineHCID 7369Benzenesulfonyl chlorideHCID 8471Triethylamine

生成物 1

HCID 8087121-(Benzenesulfonyl)piperazine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-f7a4cdc1ca104faa8100eda6e6bfe630
出典データセット
uspto-grants-2007_09
特許番号
US07265122B2

関連ノート

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