反应详情

温度

5 °C

A diethyl ether solution (50 ml) of methanesulfonic acid (32 mg, 0.302 mmol) was added at 5° C. to an acetonitrile solution (150 ml) of 2-{4-amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide (151 mg, 0.339 mmol). The resulting mixture was stirred at 5° C. for 25 minutes. Thereafter, the solvent was distilled away under reduced pressure, an appropriate amount of diethyl ether was then added to the residue, and a solid was then collected by filtration. Thereafter, ethanol (1 ml) was added to the resulting solid, and the resulting mixture was then stirred at room temperature for approximately 1 day. Thereafter, a solid was collected by filtration, and it was then dried under reduced pressure at room temperature for 1 day, so as to obtain the title compound (145 mg, 0.268 mmol).

1. distillationThereafter, the solvent was distilled away under reduced pressure
2. additionan appropriate amount of diethyl ether was then added to the residue
3. filtrationa solid was then collected by filtration
4. additionThereafter, ethanol (1 ml) was added to the resulting solid
5. stirringthe resulting mixture was then stirred at room temperature for approximately 1 day
6. filtrationThereafter, a solid was collected by filtration, and it
7. customwas then dried under reduced pressure at room temperature for 1 day