反应详情

To a solution containing methyl glycolate (2.5 mL, 32 mmol) and trifluoromethyl-sulfonic acid (150 mL) in CH2Cl2 (10 mL) was added benzyl 2,2,2-trichloro-acetimidate (7.0 mL, 37 mmol). After stirring for several min, the mixture was poured into aqueous NaHCO3 and extracted with Et2O. The organic extract was washed with saturated aqueous NaCl, dried (MgSO4) and concentrated under reduced pressure. The residue was purified by flash chromatography, eluting with a solvent gradient of 9-17% EtOAC/Hex to afford the title compound: 1H NMR CDCl3): d 7.34 (m, 5H); 4.62 (s, 2H); 4.11 (s, 2H); 3.78 (s, 3H).

1. extractionextracted with Et2O
2. extractionThe organic extract
3. washwas washed with saturated aqueous NaCl
4. dry with materialdried (MgSO4)
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by flash chromatography
7. washeluting with a solvent gradient of 9-17% EtOAC/Hex