Phosphoric Acid → HCID 86653868, compound

Participants

Reaction Steps

A free form (501 mg) of (R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methyl-2H-isoquinolin-1-one was measured in a reaction test tube, aqueous ethanol (4.3 mL, ethanol:water=8:1) was added and the mixture was completely dissolved by heating under reflux. Thereto was added aqueous phosphoric acid solution (2 mL, solution prepared by diluting commercially available 85% phosphoric acid (2.02 g) with the above-mentioned aqueous ethanol to scale up to 10 mL), and the mixture was stirred at room temperature for one day and left standing. The precipitate was collected by filtration. The obtained precipitate (302 mg) was measured in a reaction test tube, aqueous ethanol (2.4 mL, ethanol:water=6:1) was added, and the mixture was completely dissolved by heating under reflux. The mixture was stirred at room temperature for one day and left standing. The precipitate was collected by filtration and dried under reduced pressure at 50° C. for 5 hr to give the title compound (260 mg).

Provenance & Evidence