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4-Dimethylaminoacetophenone → [4-(1-{[6-(2-Methoxy-phenyl)-pyrimidin-4-yl]-hydrazono}-ethyl)-phenyl]dimethyl amine

HRID 2063613
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HRID 2063613 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[N:14]=[CH:13][N:12]=[C:11]([NH:15][NH2:16])[CH:10]=1.[CH3:17][C:18]([C:20]1[CH:25]=[CH:24][C:23]([N:26]([CH3:28])[CH3:27])=[CH:22][CH:21]=1)=O>C(O)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[N:14]=[CH:13][N:12]=[C:11]([NH:15][N:16]=[C:18]([C:20]2[CH:25]=[CH:24][C:23]([N:26]([CH3:28])[CH3:27])=[CH:22][CH:21]=2)[CH3:17])[CH:10]=1
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참가 물질

4

반응물 2

HCID 750374-DimethylaminoacetophenoneHCID 60209698[6-(2-Methoxy-phenyl)-pyrimidin-4-yl]-hydrazine

생성물 1

HCID 73320069[4-(1-{[6-(2-Methoxy-phenyl)-pyrimidin-4-yl]-hydrazono}-ethyl)-phenyl]dimethyl amine수율 70%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

[6-(2-Methoxy-phenyl)-pyrimidin-4-yl]-hydrazine (500 mg, 2.3 mmol) and 4-dimethylaminoacetophenone (380 mg, 2.3 mmol) were dissolved in 4 mL of ethanol. The resultant reaction mixture was heated in the microwave (CEM Discover, 135 C, QuickTest Method) for 3 hours. The reaction mixture was cooled to room temperature and after standing for three days yellow crystals formed. The crystalline solid was isolated by filtration and dried in vacuo to yield 580 mg (70%) of the title compound. HPLC Purity: 93%.

후처리

  1. customThe resultant reaction mixture
  2. temperaturewas heated in the microwave (CEM Discover, 135 C, QuickTest Method) for 3 hours
  3. customyellow crystals formed
  4. customThe crystalline solid was isolated by filtration
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-b903d7db47e04e34bdf80af338fc3373
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08288398B2

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