反应详情

To a solution of 2-amino-3-methyl-N-(2-morpholinoethyl)-pentanamide free base (20 g, 0.082 mol) dissolved in methanol (400 mL, 20 vol) was added 1,2-ethanedisulfonic acid dihydrate (18.6 g, 0.082 mol, 1 eq) in one portion. The homogeneous mixture quickly becomes cloudy, and after about 5 min, solids precipitate. Agitation became difficult and an additional 200 mL methanol was added to facilitate stirring. The mixture was stirred at ambient temperature for about 30 min, and then the solids were collected by vacuum filtration. The wet cake was dried in a 40° C. vacuum oven to afford 33.4 g (93% yield) of 2-amino-3-methyl-N-(2-morpholinoethyl)-pentanamide edisylate as a white solid. 1H NMR confirmed the identity and XRD pattern matches the small scale screen sample pattern.

1. customsolids precipitate
2. additionan additional 200 mL methanol was added
3. stirringThe mixture was stirred at ambient temperature for about 30 min
4. filtrationthe solids were collected by vacuum filtration
5. customThe wet cake was dried in a 40° C. vacuum oven