Sodium Hydroxide → HCID 19610613, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 0.11 g (0.27 mmol) of 3-(4-acetylamino-benzylamino)-4-(3-chlorophenylamino)-1H-pyrazolo[3,4-d]pyrimidine (Example 57), 3 ml of water and 1.5 ml of 30% sodium hydroxide solution is heated at 100° C. for 4 hours. After cooling to RT, the reaction mixture is extracted with ethyl acetate and the extract is washed with brine, dried over sodium sulfate and concentrated by evaporation in vacuo. The residue is purified by flash chromatography on silica gel having a particle size of 0.04-0.06 mm using methylene chloride/methanol mixtures (50:1 and 20:1). The product-containing fractions are concentrated by evaporation and the residue is recrystallized from ethyl acetate/hexane, yielding the title compound; m.p. 170-171° C.; EI-MS: (M)+ =365.

Provenance & Evidence