反应详情

To 80 ml of xylene, under reflux, m-trifluoromethylaniline (32.2 g) is added. Then, 29 g of phthalidyl 2-chloro-3-pyridinecarboxylate prepared in accordance with Example 1, Supra (divided in two fractions) is poured into the mixture with an interval of 15 minutes between each addition. The reaction mixture so obtained is maintained under reflux for 5 hours, and then cooled by pouring the mixture into an ice/water bath. To allow the complete crystallization of the desired product, the poured reaction mixture is maintained for 2 hours at a temperature of 0°-5° C. The precipitate is collected by filtration and dried under vacuum, at a temperature of 40° C. A yield of 34.1 g (82.3% of theory) of phthalidyl 2-(3-trifluoromethylanilino)-3-pyridinecarboxylate is obtained (m.p. 159°-162° C.). Recrystallizing the compound with 6 volumes of ethyl acetate, 28.4 g (68.5% yield) is obtained (m.p. 164°-5° C.).

1. additionis poured into the mixture with an interval of 15 minutes between each addition
2. customThe reaction mixture so obtained
3. temperatureis maintained
4. temperatureunder reflux for 5 hours
5. temperaturecooled
6. additionby pouring the mixture into an ice/water bath
7. customthe complete crystallization of the desired product
8. customthe poured reaction mixture
9. temperatureis maintained for 2 hours at a temperature of 0°-5° C
10. filtrationThe precipitate is collected by filtration
11. customdried under vacuum, at a temperature of 40° C