Sodium Hydroxide → 4-Chloro-2-methyl-2H-pyrazolo[3,4-b]pyridine

HRID 607154ノート

反応式

HRID 607154 の反応式
[CH3:1][N:2]1[CH:10]=[C:9]2[C:4]([NH:5][CH:6]=[CH:7][C:8]2=O)=[N:3]1.P(Cl)(Cl)([Cl:14])=O.[OH-].[Na+]>>[Cl:14][C:8]1[C:9]2[C:4](=[N:3][N:2]([CH3:1])[CH:10]=2)[N:5]=[CH:6][CH:7]=1

参加物

4

反応物 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 1364007322-Methyl-2,7-dihydro-pyrazolo[3,4-b]pyridin-4-one

生成物 1

HCID 668084904-Chloro-2-methyl-2H-pyrazolo[3,4-b]pyridine収率 88%

実験手順

A mixture of the product of Example 8b (0.177 g, 1.19 mmol) and phosphorus oxychloride (3 mL) was heated under reflux for 30 min and then cooled to room temperature. The reaction mixture was poured over ice, taken to pH 8 by the addition of 1N aqueous sodium hydroxide solution, and extracted with dichloromethane (3×30 mL). The combined organic phase was dried over anhydrous magnesium sulfate, filtered, and evaporated under reduced pressure to provide the title compound (0.170 g, 88% yield).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 30 min
  3. additionThe reaction mixture was poured over ice
  4. extractionextracted with dichloromethane (3×30 mL)
  5. dry with materialThe combined organic phase was dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-d59231ea5c2146ea98c4425d194d27d5
出典データセット
uspto-grants-2011_03
特許番号
US07915411B2

反応ノート

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