反应详情

With the exclusion of moisture, 62 mg (0.38 mmol) of 3-chloro-aniline hydrochloride (see Step 14.4) are added to 92 mg (0.36 mmol) of N'-[3-(4-amino-phenyl)-4-cyano-1H-pyrazol-5-yl]-N,N-dimethylformamidine in 1 ml of methanol and the reaction mixture is boiled under reflux for 28 hours. The light-yellow reaction solution is cooled, concentrated by evaporation and chromatographed (SiO2, methylene chloride/ethanol [10:1]). Crystallization from isopropanol yields 3-(4-amino-phenyl)-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine; TLC: Rf =0.33 (methylene chloride:methanol=10:1); FAB-MS: (M)+ =336; HPLC: TRet (Grad20-100)=9.2, TRet (Grad5-40)=18.8.

1. temperatureunder reflux for 28 hours
2. temperatureThe light-yellow reaction solution is cooled
3. concentrationconcentrated by evaporation
4. customchromatographed (SiO2, methylene chloride/ethanol [10:1])
5. customCrystallization from isopropanol