反应详情

A reactor vessel is charged with 3-amino-2-isopropylthiopyridine (3.0 g, 18 mmol), 2,2,2-trifluoroethanol (21 g, 210 mmol), and methanesulfonic acid (1.7 g, 18 mmol). The solution is heated to the range 65° C. to 70° C. and then t-butylnitrite (2.2 g of a 90% solution, 19 mmol) is added drop-wise to the vessel while maintaining the temperature at 65° C. to 70° C. After nitrogen evolution ceases, the solution is cooled, neutralized with aqueous saturated sodium bicarbonate solution and then extracted with MTBE. The solvent is removed by evaporation to obtain 2-isopropyl-3-(2,2,2-trifluoroethoxy)pyridine as a crude oil (4.22 g, crude yield 94%).

1. temperatureThe solution is heated to the range 65° C. to 70° C.
2. temperaturewhile maintaining the temperature at 65° C. to 70° C
3. temperatureAfter nitrogen evolution ceases, the solution is cooled
4. extractionextracted with MTBE
5. customThe solvent is removed by evaporation