Sodium Acetate → 5-(alpha,alpha,alpha-Trifluoro-m-tolyl)pyrazolo[1,5-a]pyrimidine

HRID 225287ノート

反応式

HRID 225287 の反応式
Cl[C:2]1[N:7]2[N:8]=[CH:9][CH:10]=[C:6]2[N:5]=[C:4]([C:11]2[CH:12]=[C:13]([C:17]([F:20])([F:19])[F:18])[CH:14]=[CH:15][CH:16]=2)[CH:3]=1.C([O-])(=O)C.[Na+].[H][H]>[Pd]>[F:19][C:17]([F:18])([F:20])[C:13]1[CH:14]=[CH:15][CH:16]=[C:11]([C:4]2[CH:3]=[CH:2][N:7]3[N:8]=[CH:9][CH:10]=[C:6]3[N:5]=2)[CH:12]=1

参加物

5

反応物 3

HCID 517045Sodium AcetateHCID 233298597-Chloro-5-[3-(trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 112308145-(alpha,alpha,alpha-Trifluoro-m-tolyl)pyrazolo[1,5-a]pyrimidine

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

The mixture of 1.65 g. 7-chloro-5-(α,α,α-trifluoro-m-tolyl)pyrazolo[1,5-a]pyrimidine, 0.46 g. of anhydrous sodium acetate, 0.20 g. of 10% palladium on charcoal catayst and 100 ml. of absolute alcohol is hydrogenated in a Parr apparatus beginning at 10 lbs. pressure until one equivalent of hydrogen is absorbed in about 40 minutes. The catalyst is removed by filtration and the solvent is evaporated to dryness and water is added. The solid is collected by filtration and is recrystallized from methylene chloride-hexane to yield the desired material, m.p. 117°-118° C.

後処理

  1. additionThe mixture of 1.65 g
  2. customThe catalyst is removed by filtration
  3. customthe solvent is evaporated to dryness and water
  4. additionis added
  5. filtrationThe solid is collected by filtration
  6. customis recrystallized from methylene chloride-hexane

出典と根拠

ORDレコード
ord-1fef6677952349fbb4a1cc288e37a229
出典データセット
uspto-grants-1980_11
特許番号
US04236005

反応ノート

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