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5-(4-Methoxybenzyl)-2-methylthio-4-pyrimidone → 2-[4-(5-Bromo-3-methylpyrid-2-yl)butylamino]-5-(4-methoxybenzyl)-4-pyrimidone

HRID 485658
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HRID 485658 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH3:13])[C:5]([CH2:8][CH2:9][CH2:10][CH2:11][NH2:12])=[N:6][CH:7]=1.[CH3:14][O:15][C:16]1[CH:31]=[CH:30][C:19]([CH2:20][C:21]2[C:22](=[O:29])[NH:23][C:24](SC)=[N:25][CH:26]=2)=[CH:18][CH:17]=1>N1C=CC=CC=1>[Br:1][C:2]1[CH:3]=[C:4]([CH3:13])[C:5]([CH2:8][CH2:9][CH2:10][CH2:11][NH:12][C:24]2[NH:23][C:22](=[O:29])[C:21]([CH2:20][C:19]3[CH:30]=[CH:31][C:16]([O:15][CH3:14])=[CH:17][CH:18]=3)=[CH:26][N:25]=2)=[N:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 129515135-(4-Methoxybenzyl)-2-methylthio-4-pyrimidoneHCID 130942724-(5-Bromo-3-methyl-2-pyridinyl)butylamine

생성물 1

HCID 202690722-[4-(5-Bromo-3-methylpyrid-2-yl)butylamino]-5-(4-methoxybenzyl)-4-pyrimidone수율 70.8%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

5-Bromo-2-(4-aminobutyl)-3-methylpyridine, (0.875 g) and 5-(4-methoxybenzyl)-2-methylthio-4-pyrimidone (0.786 g) were refluxed in pyridine (3 ml) for 20 hours. The pyridine was evaporated in vacuo. Residual pyridine was removed from the residue by azeotroping with water in vacuo and dried by azeotroping with ethanol. Addition of water (10 ml) and ethanol (1 ml) gave a colourless solid. This was recrystallised from ethanol and then from methanol to give 2-[4-(5-bromo-3-methylpyrid-2-yl)butylamino]-5-(4-methoxybenzyl)-4-pyrimidone (0.97 g) m.p. 149°-50° C.

후처리

  1. customThe pyridine was evaporated in vacuo
  2. customResidual pyridine was removed from the residue
  3. customby azeotroping with water in vacuo
  4. customdried
  5. customby azeotroping with ethanol
  6. additionAddition of water (10 ml) and ethanol (1 ml)
  7. customgave a colourless solid
  8. customThis was recrystallised from ethanol

출처 및 근거

ORD 기록
ord-263410d0620444c3af3be7a672c33dbe
출처 데이터셋
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04537891

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