反应详情

温度

50 °C

110 ml (110 mmol) of 1 N hydrochloric acid were added to a solution of 13 g (30.3 mmol) of (2R,3R)-2-(2-fluorophenyl)-3-[(trans-2-phenyl-1,3-dioxan-5-yl)thio]-1-(1H-1,2,4-triazol-1-yl)-2-butanol [prepared as described in Step 5(i) above] in 80 ml of toluene. The resulting mixture was heated at 50° C. for 2.5 hours. At the end of this time, the water layer was separated and the oily layer was extracted twice with dilute hydrochloric acid and then with an aqueous sodium chloride solution. The aqueous layers were combined and sodium hydrogen carbonate was carefully added thereto in small portions until bubbles of carbon dioxide were no longer detected. The resulting mixture was extracted with ethyl acetate and the extract was then concentrated under reduced pressure to afford a solid residue. This residue was collected by filtration and then washed with a small amount of ethyl acetate to afford 5.57 g (yield 55%) of the title compound as a pale brown solid.

1. customAt the end of this time, the water layer was separated
2. extractionthe oily layer was extracted twice with dilute hydrochloric acid
3. additionsodium hydrogen carbonate was carefully added
4. extractionThe resulting mixture was extracted with ethyl acetate
5. concentrationthe extract was then concentrated under reduced pressure
6. customto afford a solid residue
7. filtrationThis residue was collected by filtration
8. washwashed with a small amount of ethyl acetate