反应详情

温度

60 °C

N1-(5-Chloropyridin-2-yl)-N2-((1S,2R,4S)-4-[(dimethylamino)carbonyl]-2-{[(5-methyl-4,5,6,7-tetrahydrothiazolo[5,4-c]pyridin-2-yl)carbonyl]amino}cyclohexyl)ethanediamide (X) (6.2 g) was dissolved in methylene chloride (120 ml). To the solution, a 1 mol/L solution of p-toluenesulfonic acid in ethanol (11.28 ml) was added, and the solvent was distilled off. To the residue, 15% aqueous ethanol (95 ml) was added, and the mixture was dissolved by stirring at 60° C. Then, the mixture was cooled to room temperature and stirred for 1 day. The precipitated crystals were collected by filtration, washed with ethanol, and then dried under reduced pressure at room temperature for 2 hours to obtain the title compound (X-a) (7.4 g).

1. distillationthe solvent was distilled off
2. additionTo the residue, 15% aqueous ethanol (95 ml) was added
3. dissolutionthe mixture was dissolved
4. temperatureThen, the mixture was cooled to room temperature
5. stirringstirred for 1 day
6. filtrationThe precipitated crystals were collected by filtration
7. washwashed with ethanol
8. customdried under reduced pressure at room temperature for 2 hours