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HCID 12951525、化合物 → 2-[4-(5-Bromo-3-methylpyrid-2-yl)butylamino]-5-(4-hydroxybenzyl)-4-pyrimidone

HRID 485657
ノート
印刷プレビュー

反応式

HRID 485657 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.[OH:14][C:15]1[CH:30]=[CH:29][C:18]([CH2:19][C:20]2[C:21](=[O:28])[NH:22][C:23](SC)=[N:24][CH:25]=2)=[CH:17][CH:16]=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:23]2[NH:22][C:21](=[O:28])[C:20]([CH2:19][C:18]3[CH:29]=[CH:30][C:15]([OH:14])=[CH:16][CH:17]=3)=[CH:25][N:24]=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 12951525HCID 12951525、化合物HCID 130942724-(5-Bromo-3-methyl-2-pyridinyl)butylamine

生成物 1

HCID 202690732-[4-(5-Bromo-3-methylpyrid-2-yl)butylamino]-5-(4-hydroxybenzyl)-4-pyrimidone収率 40.6%

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-hydroxybenzyl)-2-methylthio-4-pyrimidone (0.745 g) were refluxed in pyridine (3 ml) for 24 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. Water (20 ml) was added and the pH lowered to 6 with dilute hydrochloric acid. The solid obtained was recrystallised from ethanol/water, dimethylformamide/water and finally acetic acid/water to give 2-[4-(5-bromo-3-methylpyrid-2-yl)butylamino]-5-(4-hydroxybenzyl)-4-pyrimidone (0.54 g) m.p. 232°-4° 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. additionWater (20 ml) was added
  7. customThe solid obtained
  8. customwas recrystallised from ethanol/water, dimethylformamide/water and finally acetic acid/water

出典と根拠

ORDレコード
ord-ca06fd15db644dbb97387d55c7943159
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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