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Propylamine → 5-(2,4-Dimethylphenyl)-3-methyl-2-propylaminopyrimidin-4(3H)-one

HRID 598084
ノート
印刷プレビュー

反応式

HRID 598084 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[C:9]1[C:10](=[O:18])[N:11]([CH3:17])[C:12](SC)=[N:13][CH:14]=1.[CH2:19]([NH2:22])[CH2:20][CH3:21]>>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[C:9]1[C:10](=[O:18])[N:11]([CH3:17])[C:12]([NH:22][CH2:19][CH2:20][CH3:21])=[N:13][CH:14]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 7852PropylamineHCID 589385625-(2,4-Dimethylphenyl)-3-methyl-2-(methylthio)pyrimidin-4(3H)-one

生成物 1

HCID 589385915-(2,4-Dimethylphenyl)-3-methyl-2-propylaminopyrimidin-4(3H)-one収率 67%

反応条件

温度
100 °C

実験手順

To a sealed tube was added 0.15 g (0.57 mmol) of 5-(2,4-dimethyl-phenyl)-3-methyl-2-(methylthio)pyrimidin-4(3H)-one and 3 ml (50 mmol) of propyl amine. The mixture was heated to 100° C. for 48 h. The reaction was concentrated under reduced pressure. The residue was dissolved in ethyl acetate and washed with saturated sodium bicarbonate. The organic phase was dried over magnesium sulfate. Filtration, removal of solvent and purification of the residue via biotage eluting with 50% ethyl acetate/hexanes gave 0.1 g (67%) of product.

後処理

  1. concentrationThe reaction was concentrated under reduced pressure
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with saturated sodium bicarbonate
  4. dry with materialThe organic phase was dried over magnesium sulfate
  5. filtrationFiltration, removal of solvent and purification of the residue via biotage
  6. washeluting with 50% ethyl acetate/hexanes

出典と根拠

ORDレコード
ord-a1cb67b02dcf4ee28c2e7fc328e58e58
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07897607B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート