Cesium carbonate → 2-[1-(4-Methylpiperazin-1-yl)naphthalen-2-yloxy]-1-[4-(2,3-dimethylphenyl)piperazin-1-yl]ethanone fumarate

HRID 481359노트

반응식

HRID 481359 반응식
Cl[CH2:2][C:3]([N:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([CH3:17])[C:12]=2[CH3:18])[CH2:7][CH2:6]1)=[O:4].[CH3:19][N:20]1[CH2:25][CH2:24][N:23]([C:26]2[C:35]3[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=3)[CH:29]=[CH:28][C:27]=2[OH:36])[CH2:22][CH2:21]1.[C:37](=[O:40])([O-:39])[O-].[Cs+].[Cs+]>CN(C)C=O.O>[C:27]([OH:36])(=[O:4])/[CH:28]=[CH:29]/[C:37]([OH:39])=[O:40].[CH3:19][N:20]1[CH2:21][CH2:22][N:23]([C:26]2[C:35]3[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=3)[CH:29]=[CH:28][C:27]=2[O:36][CH2:2][C:3]([N:5]2[CH2:10][CH2:9][N:8]([C:11]3[CH:16]=[CH:15][CH:14]=[C:13]([CH3:17])[C:12]=3[CH3:18])[CH2:7][CH2:6]2)=[O:4])[CH2:24][CH2:25]1

참가 물질

6

반응물 3

HCID 10796Cesium carbonateHCID 46198312-Chloro-1-(4-(2,3-dimethylphenyl)piperazin-1-yl)ethanoneHCID 190661661-(4-Methylpiperazin-1-yl)naphthalen-2-ol

생성물 1

HCID 190661832-[1-(4-Methylpiperazin-1-yl)naphthalen-2-yloxy]-1-[4-(2,3-dimethylphenyl)piperazin-1-yl]ethanone fumarate

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

Compound 36A (477 mg, 1.79 mmol) and compound 38A (370 mg; 1.52 mmol) are stirred at room temperature under a nitrogen atmosphere in dimethylformamide (15 ml) in the presence of cesium carbonate (1.25 g, 3.82 mmol) for 12 h. The reaction mixture is then diluted with water and extracted three times with ethyl acetate. The organic phases are combined and washed three times with saturated sodium chloride solution and then dried over magnesium sulfate and concentrated. The crude reaction product is purified by flash chromatography with a mixture (90/9/1) of dichloromethane/methanol/aqueous ammonia.

후처리

  1. extractionextracted three times with ethyl acetate
  2. washwashed three times with saturated sodium chloride solution
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe crude reaction product
  6. customis purified by flash chromatography with a mixture (90/9/1) of dichloromethane/methanol/aqueous ammonia

출처 및 근거

ORD 기록
ord-34a9e5af06eb46309160c79a0ae1e48a
출처 데이터셋
uspto-grants-1998_08
특허 번호
US05789412

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