Phosphorus oxychloride → 7-(3-Pyridyl)pyrazolo[1,5-a]pyrimidine-3-carbonitrile

HRID 1278213ノート

反応式

HRID 1278213 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][C:15]([C:16]([NH2:18])=O)=[C:11]3[N:10]=[CH:9][CH:8]=2)[CH:2]=1.P(Cl)(Cl)(Cl)=O>>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[N:12]3[N:13]=[CH:14][C:15]([C:16]#[N:18])=[C:11]3[N:10]=[CH:9][CH:8]=2)[CH:2]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 145018627-(Pyridin-3-yl)pyrazolo[1,5-a]pyrimidine-3-carboxamide

生成物 1

HCID 112183037-(3-Pyridyl)pyrazolo[1,5-a]pyrimidine-3-carbonitrile

実験手順

A mixture of 1.0 g. of 7-(3-pyridyl)pyrazolo[1,5-a]-pyrimidine-3-carboxamide and 5 ml. of phosphorus oxychloride is heated at reflux temperature for 3 hours. The mixture is concentrated to dryness in vacuo. The residue is dissolved in dichloromethane and washed with a saturated solution of sodium bicarbonate. The dichloromethane solution is dried over magnesium sulfate 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, m.p. 258°-260° C.

後処理

  1. additionA mixture of 1.0 g
  2. temperatureat reflux temperature for 3 hours
  3. concentrationThe mixture is concentrated to dryness in vacuo
  4. dissolutionThe residue is dissolved in dichloromethane
  5. washwashed with a saturated solution of sodium bicarbonate
  6. dry with materialThe dichloromethane solution is dried over magnesium sulfate
  7. concentrationThe eluent is concentrated
  8. additiondiluted with hexane
  9. customto give the product of the example as crystals, m.p. 258°-260° C.

出典と根拠

ORDレコード
ord-c0837f9056ba4ae48eea93e8ce96ecf2
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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