4-(3-chloro-phenylamino)-3-(4-tert-butyloxycarbonyl-piperazin-1-yl)-1H-pyrazolo[3,4-d]pyrimidine → 4-(3-chlorophenylamino)-3-(piperazin-1-yl)-1H-pyrazolo[3,4-d]pyrimidine dihydrochloride

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Reaction Steps

Under a nitrogen atmosphere, 2.0 g (4.65 mmol) of 4-(3-chloro-phenylamino)-3-(4-tert-butyloxycarbonyl-piperazin-1-yl)-1H-pyrazolo[3,4-d]pyrimidine (see Example 24) in 80 ml of dioxane and 80 ml of HCl/dioxane (4N) are stirred at 60° C. for 2 hours. Cooling and filtering yield 4-(3-chloro-phenylamino)-3-(piperazin-1-yl)-1H-pyrazolo[3,4-d]pyrimidine dihydrochloride; analysis calc. for C15H16N7Cl.2HCl (+0.14 H2O+5% dioxane): C44.93%, H 4.78%, N 22.97%, Cl 24.91%, H2O 0.68%; found C45.12%, H 4.73%, N 23.16%, Cl 24.67%, H2O 0.68%; HPLC: tRet(grad20-100/20)=8.0.

Provenance & Evidence