反应详情

To a suspension of 16-2 (1.2 g, 2.7 mmol) in CH2Cl2 (10 ml) was added DMAP (0.03 g, 0.03 mmol) and pyridine (0.4 ml, 5.4 mmol) followed by chloroacetic anhydride (0.5 g, 3.0 mmol). The reaction mixture was stirred at room temperature for 2 h before adding additional chloroacetic anhydride (0.2 g, 0.9 mmol). After stirring for an additional 10 min the solvent was removed in vacuo. The residue was partitioned between saturated aqueous NaHCO3 and EtOAc (3×30 ml). The combined organic layers were washed with water, brine and dried (Na2SO4/MgSO4). Removal of the solvent afforded the desired product 26-1 as a red powder. MS calculated: 500.2. Found 500.1

1. stirringAfter stirring for an additional 10 min the solvent
2. customwas removed in vacuo
3. customThe residue was partitioned between saturated aqueous NaHCO3 and EtOAc (3×30 ml)
4. washThe combined organic layers were washed with water, brine
5. dry with materialdried (Na2SO4/MgSO4)
6. customRemoval of the solvent