Potassium Carbonate → 4-(3,5-Dimethylpiperazin-1-yl)benzaldehyde

HRID 591642ノート

反応式

HRID 591642 の反応式
F[C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.[CH3:10][CH:11]1[CH2:16][NH:15][CH2:14][CH:13]([CH3:17])[NH:12]1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.O>[CH3:10][CH:11]1[NH:12][CH:13]([CH3:17])[CH2:14][N:15]([C:2]2[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=2)[CH2:16]1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 660562,6-DimethylpiperazineHCID 680234-Fluorobenzaldehyde

生成物 1

HCID 866620204-(3,5-Dimethylpiperazin-1-yl)benzaldehyde収率 57%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

A mixture of 4-fluorobenzaldehyde (2.0 g, 16.1 mmol), 2,6-dimethylpiperazine (2.2 g, 19.3 mmol), and K2CO3 (2.7 g, 19.3 mmol) in DMF (10 mL) was heated at 120° C. for 4 hours. Then, the reaction was diluted with H2O and extracted with EtOAc. The organics were washed with brine, dried (Na2SO4), filtered and concentrated in vacuo. Purification by flash chromatography on silica gel eluting with 3% to 10% MeOH/CH2Cl2 afforded 4-(3,5-dimethylpiperazin-1-yl)benzaldehyde (2.0 g, 57%).

後処理

  1. extractionextracted with EtOAc
  2. washThe organics were washed with brine
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customPurification by flash chromatography on silica gel eluting with 3% to 10% MeOH/CH2Cl2

出典と根拠

ORDレコード
ord-c26f7d226a024a26a95b314d497a86d9
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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