反应详情

6-{3-[3,5-Bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidin-1-yl}-4-(trifluoromethyl)nicotinic acid (1.11 g) was dissolved in methylene chloride (30 ml), and to the solution was added oxalyl chloride (0.54 ml, 6.16 mmol) and one drop of dimethylformamide at room temperature. After stirring for 5 hours, the solvent and excess oxalyl chloride were distilled off under reduced pressure. The residue was dissolved in dioxane, added with water, and then added with sodium borohydride (0.23 g) at 0° C. The mixture was stirred for 2 hours at room temperature and added with diluted hydrochloric acid. The mixture was extracted with ethyl acetate, dried over magnesium sulfate and filtered. After concentration under reduced pressure, the target compound (0.98 g) was obtained by purification with silica gel column chromatography.

1. distillationthe solvent and excess oxalyl chloride were distilled off under reduced pressure
2. dissolutionThe residue was dissolved in dioxane
3. additionadded with water
4. additionadded with sodium borohydride (0.23 g) at 0° C
5. stirringThe mixture was stirred for 2 hours at room temperature
6. additionadded with diluted hydrochloric acid
7. extractionThe mixture was extracted with ethyl acetate
8. dry with materialdried over magnesium sulfate
9. filtrationfiltered
10. concentrationAfter concentration under reduced pressure