反应详情

温度

0 °C

A 200-ml round-bottom flask is charged with conc. HCl (4 ml) and water (40 ml), and 2-(2,2,2trifluoroethoxy)aniline (3.82 g) is added. The resulting solution is cooled at a temperature of not more than 5° C. and an aqueous solution consisting of sodium nitrite (1.7 g) dissolved in water (10 ml) is added dropwise with tile temperature held at 4° C. or below, followed by stirring For one hour. In a separate step, 3-mercapto-1,2,4-triazole (4.5 g) and potassium hydroxide (2.2 g) is dissolved in water (40 ml) to give an aqueous solution which is cooled at 0° C. A preliminarily prepared diazonium salt solution is added dropwise to this aqueous solution. Thereafter, the resulting mixture is stirred at room temperature for about one hour. The organic layer is extracted with ethyl acetate, washed with water and dried. The solvent is distilled off and the resulting crude crystal is recrystallized with a mixed solvent of n-hexane and ethyl acetate; yield 4.4 g (71 %); m.p. 100°-101° C.

1. additionis added
2. temperatureThe resulting solution is cooled at a temperature of not more than 5° C.
3. additionis added dropwise with tile temperature
4. customheld at 4° C. or below
5. customto give an aqueous solution which
6. stirringThereafter, the resulting mixture is stirred at room temperature for about one hour
7. extractionThe organic layer is extracted with ethyl acetate
8. washwashed with water
9. customdried
10. distillationThe solvent is distilled off
11. customthe resulting crude crystal is recrystallized with a mixed solvent of n-hexane and ethyl acetate