反应详情

To a suspension of zinc dust (0.34 g; 5.2 mmol) in dry THF (10 mL) was added chlorotrimethylsilane (0.33 mL; 2.6 mmol) and ethyl bromodifluoroacetate (0.50 ml; 3.9 mmol), this mixture was heated under reflux for 10 min. and then cooled to RT. To the resulting mixture was added drop-wise a solution of 1-[2-(4-octyloxy-phenyl)-morpholin-4-ylmethyl]-1H-benzotriazole in THF (5 mL). After the addition is complete the resulting mixture is heated under efflux for 2 hours. After cooling to RT the reaction mixture was filtered over Kieselguhr and the filter-cake was washed with ethanol. The solvents were removed in vacuo and the residue was purified by column chromatography (SiO2, Et2O:hexanes 1:1) to afford 2,2-difluoro-3-(2-(4-octyloxy-phenyl)-morpholin-4-yl)-propionic acid ethyl ester (0.58 g).

1. temperaturethis mixture was heated
2. temperatureunder reflux for 10 min.
3. additionAfter the addition
4. temperatureis heated under efflux for 2 hours
5. temperatureAfter cooling to RT the reaction mixture
6. filtrationwas filtered over Kieselguhr
7. washthe filter-cake was washed with ethanol
8. customThe solvents were removed in vacuo
9. customthe residue was purified by column chromatography (SiO2, Et2O:hexanes 1:1)