Sodium Methoxide → 7-Methoxy-2-(trifluoromethyl)pyrazolo[1,5-a]pyridine-4-carbaldehyde

HRID 2357903ノート

反応式

HRID 2357903 の反応式
[F:1][C:2]([F:16])([F:15])[C:3]1[CH:14]=[C:6]2[C:7]([CH:12]=[O:13])=[CH:8][CH:9]=[C:10](I)[N:5]2[N:4]=1.[CH3:17][O-:18].[Na+]>CO>[F:1][C:2]([F:16])([F:15])[C:3]1[CH:14]=[C:6]2[C:7]([CH:12]=[O:13])=[CH:8][CH:9]=[C:10]([O:18][CH3:17])[N:5]2[N:4]=1

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 593892992-Trifluoromethyl-4-formyl-7-iodo-pyrazolo[1,5-a]pyridine

生成物 1

HCID 593893517-Methoxy-2-(trifluoromethyl)pyrazolo[1,5-a]pyridine-4-carbaldehyde収率 90.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The compound of Example 113 (2.97 g) was dissolved in methanol (50.0 mL). To this solution, sodium methoxide (1.42 g) was added and the mixture was stirred for 2 hours under reflux. After cooling, the solvent was evaporated. Water was added to the resulting residue and the mixture was extracted with ethyl acetate. The organic layer was washed sequentially with water and saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated and the residue was suspended in diisopropyl ether. The solid product was collected by filtration to afford the title compound as a yellowish green powder (1.93 g).

後処理

  1. temperatureunder reflux
  2. temperatureAfter cooling
  3. customthe solvent was evaporated
  4. additionWater was added to the resulting residue
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe organic layer was washed sequentially with water and saturated brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. customThe solvent was evaporated
  9. filtrationThe solid product was collected by filtration

出典と根拠

ORDレコード
ord-e4af3c76efc441d3a04a47b4939e04ee
出典データセット
uspto-grants-2010_07
特許番号
US07763617B2

反応ノート

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