1-Phenylpiperazine → 1-(But-3-yn-1-yl)-4-phenylpiperazine

HRID 375534ノート

反応式

HRID 375534 の反応式
C(OS([C:9]1[CH:14]=[CH:13][C:12](C)=[CH:11][CH:10]=1)(=O)=O)CC#C.[C:16]1([N:22]2[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]2)C=C[CH:19]=[CH:18][CH:17]=1.C(=O)(O)[O-].[Na+]>CN(C)C=O>[CH2:16]([N:22]1[CH2:27][CH2:26][N:25]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH2:24][CH2:23]1)[CH2:17][C:18]#[CH:19]

参加物

5

反応物 3

HCID 70961-PhenylpiperazineHCID 2720203-Butynyl p-toluenesulfonateHCID 516892Sodium Bicarbonate

生成物 1

HCID 189930381-(But-3-yn-1-yl)-4-phenylpiperazine収率 78.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

A mixture of but-3-ynyl-p-toluenesulfonate (8.97 g), 1-phenylpiperazine (6.49 g) and sodium bicarbonate (3.7 g) in dimethylformamide (100 mL) is stirred at 80° C. for 14 hours. The solvent is evaporated and the residue dissolved in dichloromethane, washed with water and dried over MgSO4. The solution is filtered through silica gel and the product eluted with 10% ethyl acetate/hexanes to give 6.76 g of the title compound as a white solid.

後処理

  1. customThe solvent is evaporated
  2. dissolutionthe residue dissolved in dichloromethane
  3. washwashed with water
  4. dry with materialdried over MgSO4
  5. filtrationThe solution is filtered through silica gel
  6. washthe product eluted with 10% ethyl acetate/hexanes

出典と根拠

ORDレコード
ord-1b1257d60573427cb265f52a07432601
出典データセット
uspto-grants-1996_01
特許番号
US05486517

反応ノート

読み込み中…