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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
ノート
印刷プレビュー

反応式

HRID 485658 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-263410d0620444c3af3be7a672c33dbe
出典データセット
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04537891

反応ノート

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