反应详情

To N-(3-methyl-5isoxazolyl)-4-(trifluoromethyl)nicotinamide (Compound No. 1-2, 101.7 mg, 0.37 mmol) prepared according to Example 1, carbon tetrachloride (2 ml) and N-chlorosuccinimide (64.6 mg, 0.48 mmol) were added, and the mixture was heated under reflux for 1.5 hours. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous magnesium sulfate and concentrated. The resulting residue was purified by thin layer chromatography (a developing solvent: hexane/ethyl acetate=1/1) to obtain the title compound (69.3 mg, yield 61%).

1. additionwere added
2. temperaturethe mixture was heated
3. temperatureunder reflux for 1.5 hours
4. extractionextracted with ethyl acetate
5. washThe extract was washed with brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated
8. customThe resulting residue was purified by thin layer chromatography (a developing solvent