反应详情

温度

22.5 °C

The toluenic phase of step (a) was charged into a 500 mL round-bottomed flask placed in a water/ice bath and equipped with mechanical stirrer. 12.68 mL of methanesulfonic acid were added in about 10-15 minutes, maintaining the temperature below 22° C. After the addition, the reaction mixture was stirred for 1 hour at 20-25° C. The mixture was then filtered, and the filter was washed twice with 10.1 mL of toluene. 55.38 g of wet crude product were obtained (46.40 g of dry crude, partial yield: 97.39%; 73.52% by HPLC).

1. customplaced in a water/ice bath
2. customequipped with mechanical stirrer
3. temperaturemaintaining the temperature below 22° C
4. additionAfter the addition
5. filtrationThe mixture was then filtered
6. washthe filter was washed twice with 10.1 mL of toluene