Potassium Carbonate → 4-{[4-(Propan-2-yl)piperazin-1-yl]methyl}benzaldehyde

HRID 591788ノート

反応式

HRID 591788 の反応式
BrC[CH2:3][C:4]1[CH:11]=[CH:10][C:7]([CH:8]=[O:9])=[CH:6][CH:5]=1.C([O-])([O-])=O.[K+].[K+].[CH:18]([N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1)([CH3:20])[CH3:19]>CN(C=O)C>[CH:18]([N:21]1[CH2:26][CH2:25][N:24]([CH2:3][C:4]2[CH:5]=[CH:6][C:7]([CH:8]=[O:9])=[CH:10][CH:11]=2)[CH2:23][CH2:22]1)([CH3:20])[CH3:19]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 780131-IsopropylpiperazineHCID 110851354-(2-Bromoethyl)benzaldehyde

生成物 1

HCID 866620354-{[4-(Propan-2-yl)piperazin-1-yl]methyl}benzaldehyde収率 97.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a mixture of 4-(bromoethyl)benzaldehyde (0.200 g, 1.0 mmol) and K2CO3 (0.277 g, 2.0 mmol) in DMF (5 mL) was added N-isopropylpiperazine (0.129 g, 1.0 mmol) and the reaction was stirred at room temperature for 5 hours, then concentrated in vacuo. The resulting mixture was diluted with H2O and extracted with EtOAc. The organics were washed with brine, dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to afford 4-((4-Isopropylpiperazin-1-yl)methyl)benzaldehyde (0.240 g, 97%).

後処理

  1. concentrationconcentrated in vacuo
  2. additionThe resulting mixture was diluted with H2O
  3. extractionextracted with EtOAc
  4. washThe organics were washed with brine
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-a63aa1d34ef64ad8b344a3908eb1c517
出典データセット
uspto-grants-2016_01
特許番号
US09238640B2

反応ノート

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