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

HRID 225287노트

반응식

HRID 225287 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1fef6677952349fbb4a1cc288e37a229
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04236005

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