Dimethylcarbamoyl Chloride → HCID 178484695, compound

Participants

Reaction Steps

A solution of 0.0503 ml (0.548 mmol) of dimethylcarbamoyl chloride in 0.5 ml of THF is added dropwise, with stirring, to a suspension, cooled to 0° C., of 150 mg (0.391 mmol) of 3-(4-aminomethyl-phenylamino)4-(3-chloro-phenylamino)-1H-pyrazolo-[3,4-d]pyrimidine hydrate (see Step 77.5) in 2.5 ml of THF and 0.079 ml (0.567 mmol) of triethylamine. The reaction mixture is stirred at RT for 17 hours and then filtered, and the filter residue is washed in succession with THF, water, THF and diethyl ether. 4-(3-Chloro-phenylamino)-3-[4-(dimethylamino-carbonylamino-methyl)-phenylamino]-1H-pyrazolo[3,4-d]pyrimidine having a water content of 1.22% is obtained; m.p. 238-240° C.; ESI-MS: (M+H)+=437.

Provenance & Evidence