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

HRID 2256874노트

반응식

HRID 2256874 반응식
[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

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 680234-FluorobenzaldehydeHCID 759941-Benzylpiperazine

생성물 1

HCID 27355074-(4-Benzylpiperazin-1-yl)benzaldehyde수율 98%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9c771e2a0d4e45b4b484c9c15c0cc337
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05656624

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