反应详情

温度

40 °C

To a suspension of 2-(2-hydroxyethylamino)-4-chlorobenzoic acid (5.0 g) in water (50 ml) was added lithium hydroxide (1.0 g), was further added sodium cyanate (1.05 g) with maintaining the temperature at about 40° C. The resulting solution was reacted for 2 hours, adjusting the pH 6.0-7.0 with concentrated hydrochloric acid. Then, to the reaction solution was added lithium hydroxide (1.3 g), was further added sodium cyanate (2.1 g) at the same temperature, the resulting solution was reacted for one hour. Then, the reaction mixture was reacted for further 4 hours with adjusting the pH in the same manner as above. After the reaction, to the reaction solution was added lithium hydroxide (1.7 g) and was reacted for further 3 hours. Concentrated hydrochloric acid (5 ml) was added to this reaction solution, the resulting crystal was collected by filtration to give 4.69 g of 1-(2-hydroxyethyl)-7-chloro-2,4(1H, 3H)-quinazolinedione (yield, 84.1%).

1. customThe resulting solution was reacted for 2 hours
2. customthe resulting solution was reacted for one hour
3. customThen, the reaction mixture was reacted for further 4 hours
4. customAfter the reaction
5. customwas reacted for further 3 hours
6. filtrationthe resulting crystal was collected by filtration