p-Bromobenzenesulfonyl chloride → 4-(4-BOC-piperazinosulfonyl)bromobenzene

HRID 352824ノート

反応式

HRID 352824 の反応式
C(N(C(C)C)CC)(C)C.[Br:10][C:11]1[CH:16]=[CH:15][C:14]([S:17](Cl)(=[O:19])=[O:18])=[CH:13][CH:12]=1.[C:21]([O:25][C:26]([N:28]1[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1)=[O:27])([CH3:24])([CH3:23])[CH3:22]>C(Cl)Cl>[Br:10][C:11]1[CH:16]=[CH:15][C:14]([S:17]([N:31]2[CH2:30][CH2:29][N:28]([C:26]([O:25][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:27])[CH2:33][CH2:32]2)(=[O:19])=[O:18])=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 7396p-Bromobenzenesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 143452tert-Butyl piperazine-1-carboxylate

生成物 1

HCID 166655764-(4-BOC-piperazinosulfonyl)bromobenzene

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Diisopropylethylamine (4.00 ml) was added to a solution of 4-bromobenzenesulfonyl chloride (3.00 g) and 1-(tert-butoxycarbonyl)piperazine (2.40 g) in methylene chloride (50 ml) at room temperature. After stirring at room temperature for 30 minutes, the reaction mixture was concentrated under reduced pressure. The residue thus obtained was purified by chromatography on a silica gel column (hexane:ethyl acetate=4:1→1:1), followed by reprecipitation in a hexane—methylene chloride system, whereby the title compound (4.47 g) was obtained as a colorless solid.

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customThe residue thus obtained
  3. customwas purified by chromatography on a silica gel column (hexane:ethyl acetate=4:1→1:1)
  4. customfollowed by reprecipitation in a hexane—methylene chloride system, whereby the title compound (4.47 g)
  5. customwas obtained as a colorless solid

出典と根拠

ORDレコード
ord-7d223fde63e14ff6a8cb3d0441f8c8d8
出典データセット
uspto-grants-2004_06
特許番号
US06747023B1

反応ノート

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