反应详情

With the exclusion of air, 172 mg (1.05 mmol) of 3-chloro-aniline hydrochloride (see Step 14.4) are added to 248 mg (0.70 mmol) of N'-[3-(4-tert-butoxycarbonylamino-phenyl)-4-cyano-1H-pyrazol-5-yl]-N,N-dimethylformamidine in 2 ml of methanol and the reaction mixture is boiled for 19 hours. The reaction mixture is then concentrated by evaporation and chromatographed (SiO2, methylene chloride/ethanol [20:1]). Stirring with diethyl ether/hexane yields 3-(4-tert-butoxycarbonylamino-phenyl)-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine; m.p. 165-168° C. (decomposition); FAB-MS: (M)+= 436; HPLC: TRet (Grad20-100)=15.4.

1. concentrationThe reaction mixture is then concentrated by evaporation
2. customchromatographed (SiO2, methylene chloride/ethanol [20:1])