反应详情

Triethylamine (83.68 ml) was added to a mixture composed of the above 1-(2-amino-4,6-dichloropyrimidin-5-yl)-2-(2,2-dimethyl-[1,3]dioxolan-4-yl)ethan-1-one (61.23 g), (4-methoxybenzyl)-hydrazine hydrochloride (41.50 g) produced by the method described in U.S. Patent No. U.S.2003/18197, and dichloromethane (600 ml) over 30 minutes under cooling in an ice bath. Thereafter, while the temperature of the reaction solution was gradually raised, it was stirred for 17 hours. Thereafter, a 10% citric acid aqueous solution was added to the reaction mixture, followed by extraction with dichloromethane. The organic layer was dried over anhydrous sodium sulfate and was then concentrated under reduced pressure. A 5% citric acid aqueous solution was added to the resulting residue, and the precipitate was then collected by filtration. The resultant was washed with water, so as to obtain the title compound (73.84 g) as a solid.

1. customproduced by the method
2. temperatureThereafter, while the temperature of the reaction solution was gradually raised
3. extractionfollowed by extraction with dichloromethane
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. concentrationwas then concentrated under reduced pressure
6. additionA 5% citric acid aqueous solution was added to the resulting residue
7. filtrationthe precipitate was then collected by filtration
8. washThe resultant was washed with water