Sodium Acetate → HCID 1478146、化合物
反応式
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]=1参加物
5
実験手順
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.