反应详情

Ethyl 6-[(5-chloro-2-{[(4-chloro-2-fluorophenyl)methyl]oxy}phenyl)methyl]-2-pyridinecarboxylate (2 g) was dissolved in ethanol (15 ml) at reflux. 2M Sodium hydroxide (3.4 ml) was added and the solution heated under reflux for 30 minutes. No residual starting material by HPLC. The solution was filtered and the filter washed with a mixture of hot ethanol (5 ml) and water (5 ml). The combined filtrate and wash were re-heated to reflux, and water (15 ml) added dropwise over ˜5 minutes and the clear solution allowed to cool slowly to room temperature. The product crystallised rapidly at ˜35° C. The resulting thick suspension was cooled to 20-25° C. and stirred for 1 hour. The product was isolated and washed with 1:3 ethanol:water (20 ml) and then dried overnight at 50° C. in vacuo to give the title compound (1.94 g).

1. temperatureat reflux
2. temperaturethe solution heated
3. temperatureunder reflux for 30 minutes
4. filtrationThe solution was filtered
5. washthe filter washed with a mixture of hot ethanol (5 ml) and water (5 ml)
6. washThe combined filtrate and wash
7. temperaturewere re-heated
8. temperatureto reflux
9. additionwater (15 ml) added dropwise over ˜5 minutes
10. customThe product crystallised rapidly at ˜35° C
11. temperatureThe resulting thick suspension was cooled to 20-25° C.
12. customThe product was isolated
13. washwashed with 1:3 ethanol
14. dry with materialwater (20 ml) and then dried overnight at 50° C. in vacuo