HCID 66911481, compound → Liafensine

Participants

Reaction Steps

A solution of Compound 13 (550 g, 1.0 equiv) in 1:1 MeOH/DI water (16.5 L) was passed through a 1.2 micron in-line filter. The solution was stirred at ambient temperature as a 10% aq. NaHCO3 solution was slowly added. The batch became cloudy after 350 mL of the NaHCO3 solution had been added. Seed crystals (10.5 g) were then added, and the mixture was stirred for an additional 1 hour. More of the NaHCO3 solution (4 L) was added over 40 minutes. After the addition was complete, the mixture was stirred for 2 hours and then filtered. After conditioning on the filter under N2 for 1 hour, the wet filter cake was re-suspended in 8:2 DI water/MeOH (5.5 L), stirred for 2 hours, and then filtered. The filter cake was conditioned under N2 for 48 hours and then dried in vacuo at 35° C. for 48 hours to give 450 g of the Compound 2 as a white solid in 96% yield and >99% purity.

Provenance & Evidence