HCID 59233381, compound → HCID 59233379, compound

Participants

Reaction Steps

A mixture of 4-(6-chloro-4-methoxy-pyridazin-3-ylamino)-piperidine-1-carboxylic acid tent-butyl ester (D1) (0.44 g, 1.27 mmol) and Amberlyst® 15 ion exchange resin, acidic form (4.1 mmol/g) (1.55 g, 6.35 mmol) in methanol (20 ml) was shaken at room temperature for 18 h. After this period, the mixture was filtered and then a 7M solution of ammonia in methanol was added. The mixture was shaken for 1 h, filtered and the filtrate evaporated in vacuo. The crude product was purified by flash column chromatography (silica gel; 3% ammonia in methanol (7M)/dichloromethane). The desired fractions were collected and evaporated in vacuo. to yield D2 (0.25 g, 81%) as a white solid. C10H15ClN4O requires 242; Found 243 (MH+).

Provenance & Evidence