反应详情

3.4 g (0.046 mol) of diethylamine and 4.8 g (0.47 mol) of triethylamine dissolved in 10 ml of benzene are dropped into the solution of 15.6 g (0.045 mol) of 2-[4-(5-trifluoromethyl-2-pyridyloxy)phenoxy]propionyl chloride in 40 ml of anhydrous benzene at 0°-5° C. under stirring. After termination of the portionwise addition, the reaction mixture is stirred for additional 2 hours whilst it is allowed to warm to room temperature. The mixture is filtered off, the precipitate is washed with a little volume of ether, the filtrate is washed first with 5% hydrochloric acid and then with saturated sodium chloride solution, then dried over anhydrous magnesium sulfate and finally evaporated to dryness. The crude product is purified by chromatography on a column filled with silica gel of 0.063-0.2 mm particle size by using a 4:1 mixture of n-hexane/acetone for elution.

1. additionAfter termination of the portionwise addition
2. stirringthe reaction mixture is stirred for additional 2 hours whilst it
3. filtrationThe mixture is filtered off
4. washthe precipitate is washed with a little volume of ether
5. washthe filtrate is washed first with 5% hydrochloric acid
6. dry with materialwith saturated sodium chloride solution, then dried over anhydrous magnesium sulfate
7. customfinally evaporated to dryness
8. customThe crude product is purified by chromatography on a column
9. additionfilled with silica gel of 0.063-0.2 mm particle size
10. additiona 4:1 mixture of n-hexane/acetone
11. washfor elution