反应详情

A solution of 10.6 g (0.030 mol) of (R)(+)-2-[4-(5-chloro-3-fluoropyridin-2-yloxy)-phenoxy]-propionic acid chloride in 100 ml toluene is added slowly, while stirring into a solution of 4.9 ml (0.035 mol) of triethylamine and 2 ml (0.035mol) of methanol in 40 ml of toluene, that is cooled in an ice/bath. When everything is added, the ice-bath is removed and the reaction mixture is stirred for 3 hours at room temperature. The reaction mixture is then poured into ice-water and the organic material is extracted twice with ethyl acetate. The ethyl acetate layer is washed with a saturated salt solution, dried over magnesium sulfate, filtered and evaporated. The residue is purified by chromatography over a silicagel column with a hexane/ethyl acetate solution. After evaporation of the solvent, a clear oil, the above ester remains n35D 1.5859, [α]20D =+38.8±0.5 (2 % acetone).

1. temperatureis cooled in an ice/bath
2. additionWhen everything is added
3. customthe ice-bath is removed
4. additionThe reaction mixture is then poured into ice-water
5. extractionthe organic material is extracted twice with ethyl acetate
6. washThe ethyl acetate layer is washed with a saturated salt solution
7. dry with materialdried over magnesium sulfate
8. filtrationfiltered
9. customevaporated
10. customThe residue is purified by chromatography over a silicagel column with a hexane/ethyl acetate solution
11. customAfter evaporation of the solvent