反应详情

Triphenylphosphine (22 mg) was added to a suspension of 3-(4-fluorophenyl)-3-methoxy-3-(5-{(E)-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]vinyl}-2H-[1,2,4]triazol-3-yl)propan-1-ol (38 mg) in carbon tetrachloride (2 mL) and THF (2 mL), and the reaction solution was heated under reflux for seven hours. The reaction solution was left to cool to room temperature and concentrated under reduced pressure. Ethyl acetate and a saturated sodium bicarbonate solution were added to the resulting residue, and the organic layer was separated. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (carrier: Chromatorex™ NH; elution solvent: heptane-ethyl acetate system), again purified with silica gel column chromatography (elution solvent: ethyl acetate-methanol system) and then purified by LC-MS. After concentrating the target fraction, ethyl acetate and a saturated sodium bicarbonate solution were added to the residue, and the organic layer was separated. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to obtain 0.69 mg of the title compound. The property values of the compound are as follows.

1. temperaturethe reaction solution was heated
2. temperatureunder reflux for seven hours
3. waitThe reaction solution was left
4. concentrationconcentrated under reduced pressure
5. additionEthyl acetate and a saturated sodium bicarbonate solution were added to the resulting residue
6. customthe organic layer was separated
7. washThe organic layer was washed with brine
8. dry with materialdried over anhydrous magnesium sulfate
9. concentrationconcentrated under reduced pressure
10. customThe resulting residue was purified by silica gel column chromatography (carrier: Chromatorex™ NH; elution solvent: heptane-ethyl acetate system)
11. customagain purified with silica gel column chromatography (elution solvent: ethyl acetate-methanol system)
12. custompurified by LC-MS
13. concentrationAfter concentrating the target fraction, ethyl acetate
14. additiona saturated sodium bicarbonate solution were added to the residue
15. customthe organic layer was separated
16. washThe organic layer was washed with brine
17. dry with materialdried over anhydrous magnesium sulfate
18. concentrationconcentrated under reduced pressure