Propionic Acid → HCID 15291423, compound

Participants

Reaction Steps

Into 2 ml of DMF were dissolved 200 mg (0.68 mmol) of cis-3-amino-4-methyl-1-(l-methylindazol-3-ylcarbonyl)pyrrolidine hydrochloride and 0.09 ml (0.68 mmol) of triethylamine, and the solution was stirred for 0.5 hours at room temperature. This solution was added to another solution which was separately prepared by dissolving 0.05 ml (0.68 mmol) of propionic acid and 112 mg (0.68 mmol) of CDI into 2 ml of DMF, followed by stirring for 2 hours at room temperature. Resultant mixture was stirred overnight at room temperature. After DMF was distilled off, to the residue was added water and the solution was made alkaline with sodium bicarbonate, which was then extracted with methylene chloride. After washed with saturated saline solution and dried over anhydrous magnesium sulfate, the solution was concentrated under reduced pressure to obtain crude oil. This was subjected to silica gel column chromatographic purification (methylene chloride:acetone=5:1) to obtain 37 mg (17.3%) of aimed compound. m.p. 139°-141° C.

Provenance & Evidence