Hydrochloric Acid → 6-Amino-2-[5-fluoro-1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-7-(2,2,2-trifluoroethyl)-7,9-dihydro-8H-purin-8-one

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Reaction Conditions

Reaction Steps

Under an argon atmosphere, 5.005 g (6.458 mmol) of the compound from example 32A were dissolved in 355 ml of tetrahydrofuran and cooled to 0° C., and 16.145 ml (16.145 mmol) of a 1N solution of bis(trimethylsilyl)sodium amide in tetrahydrofuran were added dropwise. The mixture was stirred at 0° C. for 2 h and then at RT for 16 h. 16.145 ml (16.145 mmol) of 1N hydrochloric acid were added and the mixture was concentrated on a rotary evaporator. The residue was taken up in ethyl acetate and the organic phase was washed twice with water, dried over sodium sulfate and concentrated on a rotary evaporator. 6.13 g of the title compound were obtained (purity by HPLC 61%). 500 mg of residue were purified by means of preparative HPLC (eluent: methanol/water, gradient 30:70→90:10). 93 mg of the title compound were obtained (36% of theory).

Provenance & Evidence