反应详情

温度

59 °C

At 50° C., 1.77 ml (22.81 mmol) of methanesulfonyl chloride are added dropwise to a solution of 1.30 g (8.77 mmol) of 3-methyl-1H-pyrrolo[2,3-b]pyridine 7-oxide in 7.5 ml of DMF such that the temperature increases to 59° C. The mixture is then stirred at 70° C. for 4 h. After cooling to room temperature, 30 ml of water are added slowly, at 5° C., the pH is adjusted to 10 by addition of 20% strength sodium hydroxide solution and the mixture is stirred for another hour. The precipitated solid is filtered off, washed with water and then dried under reduced pressure.

1. temperatureAfter cooling to room temperature
2. stirringthe mixture is stirred for another hour
3. filtrationThe precipitated solid is filtered off
4. washwashed with water
5. customdried under reduced pressure