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

HRID 1447888

反応式

HRID 1447888 の反応式
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]([NH2:20])=O)=[C:13]3[N:12]=[CH:11][CH:10]=2)[CH:4]=1.P(Cl)(Cl)(Cl)=O>>[F:21][C:2]([F:1])([F:22])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]#[N:20])=[C:13]3[N:12]=[CH:11][CH:10]=2)[CH:4]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 27776927-[3-(Trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carboxamide

生成物 1

HCID 27410147-[3-(Trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carbonitrile

実験手順

One gram of 7-(α,α,α-trifluoro-m-tolyl)pyrazolo[1,5-a]pyrimidine-3-carboxamide and 5 ml. of phosphorus oxychloride is refluxed for 3 hours. The reaction mixture is evaporated to dryness and the residue is dissolved in methylene chloride, washed with saturated sodium bicarbonate solution, dried with anhydrous sodium sulfate. After passing through a short pad of hydrous magnesium silicate with eluent methylene chloride. Concentration of the eluent with addition of n-hexane gives the product, m.p. 141°-143° C.

後処理

  1. customThe reaction mixture is evaporated to dryness
  2. dissolutionthe residue is dissolved in methylene chloride
  3. washwashed with saturated sodium bicarbonate solution
  4. dry with materialdried with anhydrous sodium sulfate
  5. additionConcentration of the eluent with addition of n-hexane
  6. customgives the product, m.p. 141°-143° C.

出典と根拠

ORDレコード
ord-67ede502dbfe46ea9f2258b8197708ba
出典データセット
uspto-grants-1979_12
特許番号
US04178449

関連ノート

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