Triethylamine → HCID 4634543、化合物

HRID 390990ノート

反応式

HRID 390990 の反応式
[C:1]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].C(N(CC)CC)C.[F:21][C:22]1[CH:27]=[CH:26][C:25]([S:28](Cl)(=[O:30])=[O:29])=[CH:24][CH:23]=1>C(Cl)Cl>[C:4]([O:3][C:1]([N:8]1[CH2:9][CH2:10][N:11]([S:28]([C:25]2[CH:26]=[CH:27][C:22]([F:21])=[CH:23][CH:24]=2)(=[O:30])=[O:29])[CH2:12][CH2:13]1)=[O:2])([CH3:7])([CH3:6])[CH3:5]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 95884-Fluorobenzenesulfonyl chlorideHCID 143452tert-Butyl piperazine-1-carboxylate

生成物 1

HCID 4634543HCID 4634543、化合物収率 101.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To N-Boc-piperazine (500 mg) in DCM (10 ml) was added triethylamine (450 μl) and 4-fluorobenzenesulfonyl chloride (564 mg). The reaction mixture was stirred at room temperature overnight, then partitioned between dichloromethane and water, washed with brine, organics were dried over MgSO4, filtered and volatiles removed in vacuo to give 4-(4-fluoro-benzenesulfonyl)-piperazine-1-carboxylic acid tert-butyl ester (937 mg).

後処理

  1. custompartitioned between dichloromethane and water
  2. washwashed with brine
  3. dry with materialorganics were dried over MgSO4
  4. filtrationfiltered
  5. customvolatiles removed in vacuo

出典と根拠

ORDレコード
ord-e390d515d57947cfac7b5041c1014283
出典データセット
uspto-grants-2013_02
特許番号
US08383620B2

反応ノート

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