反应详情

With the exclusion of air, 16.2 9 (46.6 mmol) of N′-[3-(4-tert-butoxycarbonyl-piperazin-1 -yl)-4-cyano-1H-pyrazol-5-yl]-N,N-dimethyl-formamidine in 130 ml methanol are heated to boiling with 11.47 g (70 mmol) of 3-chloro-aniline hydrochloride. After 9 hours the reaction mixture is cooled, filtered and washed with methanol and DIPE. Stirring the crude product in boiling ethanol, cooling and filtration yield 4-(3-chloro-phenylamino)-3-(4-tert-butyloxycarbonyl-piperazin-1-yl)-1H-pyrazolo[3,4-d]pyrimidine; HPLC: tRet(grad20-100/20)=15.7; IR (KBr) interalia 1706 s, 1631 s, 1610 s, 1589 s, 1508 m, 1482 s, 1425 m, 1364 m, 1304 m, 1283 m, 1245 m, 1170 m, 1122 m.

1. temperatureAfter 9 hours the reaction mixture is cooled
2. filtrationfiltered
3. washwashed with methanol and DIPE
4. temperaturecooling
5. filtrationfiltration