反应详情

To a solution of 2-amino-3-methyl-N-(2-morpholinoethyl)-pentanamide free base (25 g, 0.103 mol) dissolved in absolute, anhydrous ethanol (250 mL, 10 vol) cooled in an ice-water bath was slowly added concentrated sulfuric acid (4 mL, 75 mmol) by dropwise addition. Precipitation immediately occurred causing stirring to stop. The ice-water bath was removed and the addition of ethanol (200 mL) and isopropanol (225 mL) was necessary to restart stirring. The remaining required sulfuric acid (7 mL, 131 mmol) was slowly added in an ethanol:isopropanol solution (2:1, 75 mL). An exotherm (20.8° C.-24.0° C.) was observed. The white slurry was allowed to stir overnight under positive nitrogen pressure. The mixture was then filtered washing with isopropanol (150 mL) and dried under high vacuum (35° C.-40° C.) to afford 33.6 g (75% yield) of 2-amino-3-methyl-N-(2-morpholinoethyl)-pentanamide Disulfate as a white solid. 1H NMR, LC-MS confirmed the identity and XRD pattern matches the small scale screen sample pattern.

1. temperaturecooled in an ice-water bath
2. additionby dropwise addition
3. customPrecipitation
4. customThe ice-water bath was removed
5. additionthe addition of ethanol (200 mL) and isopropanol (225 mL)
6. stirringto restart stirring
7. customAn exotherm (20.8° C.-24.0° C.)
8. stirringto stir overnight under positive nitrogen pressure
9. filtrationThe mixture was then filtered
10. washwashing with isopropanol (150 mL)
11. customdried under high vacuum (35° C.-40° C.)