Benzenemethanamine, 3-chloro- → HCID 178483760, compound

Participants

Reaction Conditions

Reaction Steps

The mixture of N′-[3-(2-methanesulfonyl-pyrimidin-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-6-yl]-N,N-dimethyl-ethane-1,2-diamine (from Example 23 supra) (160 mg, crude) and 3-chlorobenzylamine (236 mg, 1.67 mmol) was heated at 130° C. with stirring for 3 hours. The resulting oil was purified by chromatography (silica gel, 7 g, 200-300 mesh, eluting with dichloromethane:methanol, 10:1) and further purified by prep-HPLC. Concentrated HCl was added to the fractions with product and concentrated under reduced pressure to give N-{3-[2-(3-chloro-benzylamino)-pyrimidin-4-yl]-1H-pyrazolo[3,4-d]pyrimidin-6-yl}-N′,N′-dimethyl-ethane-1,2-diamine; hydrochloride. (Yield 26 mg).

Provenance & Evidence