反应详情

5-Chloro-1,3-dimethylpyrazole-4-carboxylic acid (349 mg, 2 mmol) was dissolved in thionyl chloride (10 ml), and the solution was stirred at reflux temperature for 2 hours. After concentration under reduced pressure, the resulting acid chloride was added to a solution of 2-(1,4-dimethylpentyl)-4-[2,2,2-trifluoro-1-(trifluoromethyl)ethyl]aniline (682 mg, 2 mmol) and triethylamine (300 mg, 3 mmol) in tetrahydrofuran (20 ml) under ice-cooling, and the resulting mixture was stirred at reflux temperature for 2 hours. The reaction mixture was diluted with ethyl acetate and then washed with water. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure, and the resulting residue was separated and purified by silica gel column chromatography (hexane:ethyl acetate=2:3) to obtain 200 mg of the desired compound.

1. temperatureat reflux temperature for 2 hours
2. concentrationAfter concentration under reduced pressure
3. temperaturecooling
4. stirringthe resulting mixture was stirred
5. temperatureat reflux temperature for 2 hours
6. washwashed with water
7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. customthe resulting residue was separated
10. custompurified by silica gel column chromatography (hexane:ethyl acetate=2:3)