反应详情

(2S,5R)-tert-butyl 5-(allyloxy(tert-butoxycarbonyl)amino)-2-carbamoyl-4-(methoxymethyl)-5,6-dihydropyridine-1(2H)-carboxylate (Intermediate 73, 3.07 g, 6.95 mmol) was dissolved in 20 mL DCM. Then 5.36 mL TFA was added dropwise at 0° C. The mixture was stirred at rt for 3 h. The solvent was removed in vacuo and co-evaporated twice with 5 mL MeOH. The residue was dissolved in MeOH (10 mL) and ammonium hydroxide (30% in water) was added until it was basic. The mixture was rotovapored at rt and the residue was freeze-dried over night to give a solid. It was dissolved in DCM and purified on silica gel eluting with 0-100% MeOH/DCM to give a off-white solid (1.12 g, 66.8%).

1. customThe solvent was removed in vacuo
2. dissolutionThe residue was dissolved in MeOH (10 mL)
3. additionammonium hydroxide (30% in water) was added until it
4. customwas rotovapored at rt
5. customthe residue was freeze-dried over night
6. customto give a solid
7. custompurified on silica gel eluting with 0-100% MeOH/DCM