反应详情

With the exclusion of air, 1.86 g (7.49 mmol) of N′-[3-(morpholin-4-yl)-4-cyano-1 H-pyrazol-5-yl]-N,N-dimethyl-formamidine in 45 ml of methanol are heated to boiling with 1.84 g (11.2 mmol) of 3-chloro-aniline hydrochloride, during which the solid temporarily dissolves. After about 30 min, a precipitate separates out again. After 8 hours the reaction mixture is cooled, filtered and washed with methanol and DIPE. Stirring the crude product in a boiling mixture of 40 ml of ethanol, 20 ml of chloroform and 20 ml of dioxane yields 4-(3-chloro-phenylamino)-3-(morpholin-4-yl)-1H-pyrazolo[3,4-d]pyrimidine; m.p. 275-276° C.; HPLC:tRet(grad20-100/20)=11.6.

1. dissolutiontemporarily dissolves
2. temperatureAfter 8 hours the reaction mixture is cooled
3. filtrationfiltered
4. washwashed with methanol and DIPE
5. additionin a boiling mixture of 40 ml of ethanol, 20 ml of chloroform and 20 ml of dioxane