反应详情

温度

5 °C

An acetone solution (50 ml) of ethane-1,2-disulfonate (70 mg, 0.368 mmol) was added at 5° C. to an acetone solution (50 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 (164 mg, 0.368 mmol). The resulting mixture was stirred at 5° C. for 20 minutes. Thereafter, the reaction solution was left at rest at 5° C. for 18 hours, and it was then stirred at room temperature for 7 hours. Thereafter, the precipitated solid was collected by filtration, and it was then dried under reduced pressure at room temperature for approximately 1 day, so as to obtain the title compound (119 mg, 0.187 mmol).

1. waitThereafter, the reaction solution was left at rest at 5° C. for 18 hours
2. stirringit was then stirred at room temperature for 7 hours
3. filtrationThereafter, the precipitated solid was collected by filtration, and it
4. customwas then dried under reduced pressure at room temperature for approximately 1 day