反应详情

A solution of the 2-(4-((3-chloro-5-(trifluoromethyl)-2-pyridinyl)oxy)phenoxy)propionyl chloride (prepared in Step A) in 50 ml of acetonitrile was added to a mixture of 3.82 g (19.4 mmol) of 4-aminobenzotrifluoride, hydrochloride and 4.90 g (48.4 mmol) of triethylamine in 25 ml of acetonitrile. The reaction mixture was warmed at reflux for 4.0 hours and then poured over crushed ice. The resulting precipitate was collected by filtration and dried. The residual solid was recrystallized from methylcyclohexane to give 9.1 g (93 percent of theoretical) of the above-named product as a tan solid which melted at 140°-143° C. The structure of the product was confirmed by its IR and NMR spectrum. (Compound 1)

1. temperatureThe reaction mixture was warmed
2. temperatureat reflux for 4.0 hours
3. additionpoured
4. customover crushed ice
5. filtrationThe resulting precipitate was collected by filtration
6. customdried
7. customThe residual solid was recrystallized from methylcyclohexane