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

HRID 1278213노트

반응식

HRID 1278213 반응식
[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

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-c0837f9056ba4ae48eea93e8ce96ecf2
출처 데이터셋
uspto-grants-1981_07
특허 번호
US04281000

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