反应详情

Ammonium chloride (1.10 g), WSC.HCl (2.97 g), HOBt.H2O (2.37 g), and diisopropylethylamine (7.06 ml) were added to a DMF solution (40 ml) containing 6-(cis-2-(tert-butoxycarbonylamino)cyclohexylamino)-2-chloro-5-fluoronicotinic acid (2.00 g), followed by stirring at room temperature for 7 hours. A saturated aqueous ammonium chloride solution, water, and ethyl acetate were added to the reaction mixture. The organic layer was collected, washed with saturated saline, and dried over anhydrous magnesium sulfate, and the solvent was distilled away under reduced pressure. Diisopropylether was added to the obtained residue, solid matter was collected by filtration, and a white solid of tert-butyl cis-2-(5-aminocarbonyl-6-chloro-3-fluoropyridin-2-ylamino)cyclohexylcarbamate (1.75 g) was thus obtained.

1. customThe organic layer was collected
2. washwashed with saturated saline
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationthe solvent was distilled away under reduced pressure
5. additionDiisopropylether was added to the obtained residue, solid matter
6. filtrationwas collected by filtration