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Trifluoroacetic acid → 1-{4-[4-(3,5-Dimethylpyridin-2-yl)piperazine-1-carbonyl]phenyl}-5-methylimidazolidin-2-one

HRID 2411777
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HRID 2411777 반응식
[CH3:1][C:2]1[C:3]([N:9]2[CH2:14][CH2:13][N:12]([C:15]([C:17]3[CH:22]=[CH:21][C:20]([N:23]4[CH:27]([CH3:28])[CH2:26][N:25](CC5C=CC(OC)=CC=5)[C:24]4=[O:38])=[CH:19][CH:18]=3)=[O:16])[CH2:11][CH2:10]2)=[N:4][CH:5]=[C:6]([CH3:8])[CH:7]=1.FC(F)(F)C(O)=O>ClCCl>[CH3:1][C:2]1[C:3]([N:9]2[CH2:10][CH2:11][N:12]([C:15]([C:17]3[CH:18]=[CH:19][C:20]([N:23]4[CH:27]([CH3:28])[CH2:26][NH:25][C:24]4=[O:38])=[CH:21][CH:22]=3)=[O:16])[CH2:13][CH2:14]2)=[N:4][CH:5]=[C:6]([CH3:8])[CH:7]=1
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참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 712522003-{4-[4-(3,5-Dimethylpyridin-2-yl)piperazine-1-carbonyl]phenyl}-1-(4-methoxybenzyl)-4-methylimidazolidin-2-one

생성물 1

HCID 712528351-{4-[4-(3,5-Dimethylpyridin-2-yl)piperazine-1-carbonyl]phenyl}-5-methylimidazolidin-2-one수율 106.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-{4-[4-(3,5-dimethylpyridin-2-yl)piperazine-1-carbonyl]phenyl}-1-(4-methoxybenzyl)-4-methylimidazolidin-2-one (105 mg) described in Example 420 was dissolved in dichloromethane (1 mL), trifluoroacetic acid (2 mL) was added, and the mixture was stirred at room temperature overnight. The solvent was evaporated from the reaction mixture, 5% aqueous sodium hydrogen carbonate solution was added, and the mixture was extracted with chloroform/methanol (10/1). The organic layer was dried over sodium sulfate, and the solvent was evaporated. The obtained residue was suspension washing with IPE to give the title compound (86 mg).

후처리

  1. customThe solvent was evaporated from the reaction mixture, 5% aqueous sodium hydrogen carbonate solution
  2. additionwas added
  3. extractionthe mixture was extracted with chloroform/methanol (10/1)
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. customthe solvent was evaporated
  6. washwashing with IPE

출처 및 근거

ORD 기록
ord-e8a930c054cd48afa19bcd633beb4d82
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08816079B2

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