Dimethylformamide → HCID 21163078、化合物

HRID 1278202ノート

反応式

HRID 1278202 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[N:12]3[N:13]=[CH:14][CH:15]=[C:11]3[N:10]=[CH:9][CH:8]=2)[CH:2]=1.P(Cl)(Cl)(Cl)=O.[OH-].[Na+].CN(C)[CH:25]=[O:26]>>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[N:12]3[N:13]=[CH:14][C:15]([CH:25]=[O:26])=[C:11]3[N:10]=[CH:9][CH:8]=2)[CH:2]=1

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 11206374HCID 11206374、化合物

生成物 1

HCID 21163078HCID 21163078、化合物

実験手順

A 1.0 g. sample of 7-(3-pyridyl)pyrazolo[1,5-a]-pyrimidine is added to an ice cold solution of 1.0 ml. of phosphorus oxychloride in 3 ml. of N,N-dimethylformamide. The reaction mixture is heated on a steam bath for 3 hours and poured into ice. The mixture is made basic with a solution of sodium hydroxide and extracted into dichloromethane. The dichloromethane solution is washed with water and passed through a column of hydrous magnesium silicate. The eluent is concentrated and diluted with hexane to give the product of the example as crystals.

後処理

  1. temperatureThe reaction mixture is heated on a steam bath for 3 hours
  2. additionpoured into ice
  3. extractionextracted into dichloromethane
  4. washThe dichloromethane solution is washed with water
  5. concentrationThe eluent is concentrated
  6. additiondiluted with hexane
  7. customto give the product of the example as crystals

出典と根拠

ORDレコード
ord-3a359b6a09454a2d882ee0575e376313
出典データセット
uspto-grants-1981_07
特許番号
US04281000

反応ノート

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