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Sodium Acetate → HCID 1478146, 화합물

HRID 1707066
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HRID 1707066 반응식
Cl[C:2]1[N:7]2[N:8]=[CH:9][N:10]=[C:6]2[N:5]=[C:4]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([F:20])([F:19])[F:18])[CH:12]=2)[CH:3]=1.C([O-])(=O)C.[Na+]>[Pd].C(O)C>[F:20][C:17]([F:18])([F:19])[C:13]1[CH:12]=[C:11]([C:4]2[CH:3]=[CH:2][N:7]3[N:8]=[CH:9][N:10]=[C:6]3[N:5]=2)[CH:16]=[CH:15][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 517045Sodium AcetateHCID 203333567-Chloro-5-[3-(trifluoromethyl)phenyl][1,2,4]triazolo[1,5-a]pyrimidine

생성물 1

HCID 1478146HCID 1478146, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

A mixture of 0.30 g. of 7-chloro-5-(m-trifluoromethylphenyl)-1,2,4-triazolo[1,5-a]pyrimidine, 0.10 g. of 10% palladium on charcoal catalyst, and 0.09 g. of anhydrous sodium acetate in 100 ml. of absolute ethanol is hydrogenated at 10 lbs. pressure for 30 minutes. The solution is filtered through a Celite pad and then evaporated to dryness. A methylene chloride solution of this material is washed with an aqueous saturated sodium bicarbonate solution. The organic layer, after drying with anhydrous magnesium sulfate, is passed through a short pad of hydrous magnesium silicate. The eluent is refluxed and the gradual addition of hexane caused the desired compound to crystallize to give product, m.p. 201°-202° C.

후처리

  1. additionA mixture of 0.30 g
  2. filtrationThe solution is filtered through a Celite pad
  3. customevaporated to dryness
  4. washA methylene chloride solution of this material is washed with an aqueous saturated sodium bicarbonate solution
  5. dry with materialThe organic layer, after drying with anhydrous magnesium sulfate
  6. temperatureThe eluent is refluxed
  7. additionthe gradual addition of hexane
  8. customto crystallize
  9. customto give product, m.p. 201°-202° C.

출처 및 근거

ORD 기록
ord-328ba923a2dd47f49d0d1b5545fc506e
출처 데이터셋
uspto-grants-1980_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04209621

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