反应详情

A mixture of 94 g (245.1 mmol) of 3-[4-(N-Boc-aminomethyl)-phenylamino]-4-cyano-5-dimethylamino-methyleneamino-pyrazole, 44.2 g (269.4 mmol) of 3-chloro-aniline hydrochloride [for preparation see: Justus Liebigs Ann. Chem. 176, 45 (1875)] and 1000 ml of ethanol is heated under reflux for 60 hours and then concentrated by evaporation in vacuo. The residue is dissolved in ethyl acetate, and the organic phase is washed with ice-cold 0.5N hydrochloric acid, water and brine, dried over sodium sulfate and concentrated by evaporation in vacuo. After recrystallization of the residue from ethyl acetate/hexane and from methanolimethylene chloride, 3-[4-(N-Boc-aminomethyl)-phenylamino]-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine is obtained; m.p. 196° C.; ESI-MS: (M−H)−=464.

1. temperatureis heated
2. temperatureunder reflux for 60 hours
3. concentrationconcentrated by evaporation in vacuo
4. dissolutionThe residue is dissolved in ethyl acetate
5. washthe organic phase is washed with ice-cold 0.5N hydrochloric acid, water and brine
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated by evaporation in vacuo
8. customAfter recrystallization of the residue from ethyl acetate/hexane