Potassium Carbonate → 4-(4-Benzylpiperazin-1-yl)benzaldehyde

HRID 2256874ノート

反応式

HRID 2256874 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.F[C:15]1[CH:22]=[CH:21][C:18]([CH:19]=[O:20])=[CH:17][CH:16]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([C:15]2[CH:22]=[CH:21][C:18]([CH:19]=[O:20])=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 680234-FluorobenzaldehydeHCID 759941-Benzylpiperazine

生成物 1

HCID 27355074-(4-Benzylpiperazin-1-yl)benzaldehyde収率 98%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Heat a mixture of 4-benzylpiperazine (5.0 mL, 28.8 mmol), 4-flurobenzaldehyde (3.1 mL, 28.8 mmol)) and anhydrous K2CO3 (5.96 g, 43.1 mmol)) in DMF (50 mL) to -150° C. overnight. Cool the mixture to room temperature, partition between water and ether (Et2O), and extract with Et2O. Combine the Et2O extracts, wash with water and brine, dry over anhydrous Na2SO4 and concentrate in vacuo to obtain 7.91 g (98%) of 4-(4-benzylpiperazin-1-yl)benzaldehyde as a yellow solid of sufficient purity to be employed in Example 1 without further purification.

後処理

  1. temperatureHeat
  2. custompartition between water and ether (Et2O)
  3. extractionextract with Et2O
  4. washwash with water and brine
  5. dry with materialdry over anhydrous Na2SO4
  6. concentrationconcentrate in vacuo

出典と根拠

ORDレコード
ord-9c771e2a0d4e45b4b484c9c15c0cc337
出典データセット
uspto-grants-1997_08
特許番号
US05656624

反応ノート

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