Hydrochloric Acid → HCID 57961661, compound

Participants

Reaction Steps

To a solution of N-(3-aminobenzyl)-N′-(2,5-dichloropyrimidin-4-yl)benzene-1,3-diamine (900 mg, 2.0 mmol) in 2-methoxyethanol (18 mL) was added 4.00 M of hydrogen chloride in 1,4-dioxane (1.88 mL). The resultant mixture was heated at 150° C. in the microwave for 5 min. After cooling, water and NaOH (12 N) were added to neutralize the mixture to pH=7. The aqueous layer was extracted with EtOAc four times. The combined organic layers were dried, filtered and concentrated. The residue was purified by silica gel column chromatography to give the desired product as an off-white powder (66 mg, 8%). LCMS for C17H15ClN5 (M+H)+: m/z=324.0.

Provenance & Evidence