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Phosphorus oxychloride → 1-chloro-6-methyl-N-(3-(6-(methylamino)pyrimidin-4-yl)pyridin-2-yl)isoquinolin-5-amine

HRID 2092289
ノート
印刷プレビュー

反応式

HRID 2092289 の反応式
[CH3:1][C:2]1[C:3]([NH:13][C:14]2[C:19]([C:20]3[CH:25]=[C:24]([NH:26][CH3:27])[N:23]=[CH:22][N:21]=3)=[CH:18][CH:17]=[CH:16][N:15]=2)=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=O)[NH:7][CH:6]=[CH:5]2.O=P(Cl)(Cl)[Cl:30]>>[Cl:30][C:8]1[C:9]2[CH:10]=[CH:11][C:2]([CH3:1])=[C:3]([NH:13][C:14]3[C:19]([C:20]4[CH:25]=[C:24]([NH:26][CH3:27])[N:23]=[CH:22][N:21]=4)=[CH:18][CH:17]=[CH:16][N:15]=3)[C:4]=2[CH:5]=[CH:6][N:7]=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 24813Phosphorus oxychlorideHCID 589422616-methyl-5-(3-(6-(methylamino)pyrimidin-4-yl)pyridin-2-ylamino)isoquinolin-1(2H)-one

生成物 1

HCID 589422651-chloro-6-methyl-N-(3-(6-(methylamino)pyrimidin-4-yl)pyridin-2-yl)isoquinolin-5-amine

反応条件

温度
120 °C

実験手順

6-Methyl-5-(3-(6-(methylamino)pyrimidin-4-yl)pyridin-2-ylamino)isoquinolin-1(2H)-one (195 mg, 0.54 mmol) was suspended in POCl3 (10 mL) and heated at 120° C. for 3 h. POCl3 was removed in vacuo and the residue was washed with toluene three times. The residue was added to water and the resulting solid collected by filtration, washing with saturated aqueous sodium bicarbonate and water. The resulting title compound was dried in vacuo. MS (M+H)+ 377.

後処理

  1. customPOCl3 was removed in vacuo
  2. washthe residue was washed with toluene three times
  3. additionThe residue was added to water
  4. filtrationthe resulting solid collected by filtration
  5. washwashing with saturated aqueous sodium bicarbonate and water
  6. dry with materialThe resulting title compound was dried in vacuo

出典と根拠

ORDレコード
ord-5c6a0c6a745c486790d83a8708317714
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08440674B2

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