Acetyl chloride → 4-(4-Acetyl-3,5-dimethylpiperazin-1-yl)benzaldehyde

HRID 591643노트

반응식

HRID 591643 반응식
[CH3:1][CH:2]1[NH:7][CH:6]([CH3:8])[CH2:5][N:4]([C:9]2[CH:16]=[CH:15][C:12]([CH:13]=[O:14])=[CH:11][CH:10]=2)[CH2:3]1.CCN(CC)CC.[C:24](Cl)(=[O:26])[CH3:25]>C(Cl)Cl>[C:24]([N:7]1[CH:2]([CH3:1])[CH2:3][N:4]([C:9]2[CH:16]=[CH:15][C:12]([CH:13]=[O:14])=[CH:11][CH:10]=2)[CH2:5][CH:6]1[CH3:8])(=[O:26])[CH3:25]

참가 물질

5

반응물 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 866620204-(3,5-Dimethylpiperazin-1-yl)benzaldehyde

생성물 1

HCID 866620144-(4-Acetyl-3,5-dimethylpiperazin-1-yl)benzaldehyde수율 83.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 4-(3,5-dimethylpiperazin-1-yl)benzaldehyde (1.0 g, 4.6 mmol.) in CH2Cl2 (15 mL) was cooled to 0° C. and treated with Et3N (0.64 mL, 4.6 mmol) followed by acetyl chloride (0.33 mL, 4.6 mmol). The reaction stirred for 30 minutes, then concentrated in vacuo. Purification by flash chromatography on silica gel, eluting with 0% to 50% EtOAc/CH2Cl2, afforded 4-(4-acetyl-3,5-dimethylpiperazin-1-yl)benzaldehyde (1.0 g, 83%).

후처리

  1. concentrationconcentrated in vacuo
  2. customPurification by flash chromatography on silica gel
  3. washeluting with 0% to 50% EtOAc/CH2Cl2

출처 및 근거

ORD 기록
ord-8aab3bd97e3c4644856e4e4ab86b9e9c
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238640B2

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