反应详情

A mixture of 2-(tert-butoxycarbonyloxy)-5-(N-(cyclopropylmethyl)-methylsulfonamido)benzoic acid (0.300 g, 0.778 mmol), benzyl 2-hydroxyacetate (0.129 g, 0.778 mmol), EDC (0.448 g, 2.335 mmol) and DMAP (0.048 g, 0.389 mmol) in DCM (30 ml) was stirred at RT overnight. The reaction mixture was washed twice with HCl 1N and then with NaHCO3 5%. The organic phase was dried over Na2SO4, and the solvent was removed under vacuum. The crude was purified by filtration on silica gel cartridge (petroleum ether:EtOAc=80:20 to 70:30) to give 2-(benzyloxy)-2-oxoethyl 2-(tert-butoxycarbonyloxy)-5-(N-(cyclopropylmethyl)methylsulfonamido)benzoate (0.288 g, 0.540 mmol, 69.3% yield, MS/ESI+ 555.96 [MNa]+).

1. washThe reaction mixture was washed twice with HCl 1N
2. dry with materialThe organic phase was dried over Na2SO4
3. customthe solvent was removed under vacuum
4. filtrationThe crude was purified by filtration on silica gel cartridge (petroleum ether:EtOAc=80:20 to 70:30)