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

HRID 225275

反応式

HRID 225275 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-b6ae1a74f7da4a72b8218ea4820892f8
出典データセット
uspto-grants-1980_11
特許番号
US04236005

関連ノート

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