反应详情

1.41 kg of valeroamidine and 1.41 kg of diethyl acetylsuccinate were dissolved in 4.5 L of methanol and 1.16 kg of potassium hydroxide was added thereto. The mixture was stirred for 15 hours at room temperature, and then 14 L of water was added while stirring. The obtained solid was filtered, dried, and dissolved in 6 L of ethanol. Then, 840 g of thionyl chloride was added by drop for 2 hours and stirred for 12 hours at 60° C. To this mixture was added a solution of 1.22 kg of sodium bicarbonate in 15 L of water and the produced solid was filtered and dried to obtain 1.35 kg (47.8% yield) of the titled compound.

1. stirringwhile stirring
2. filtrationThe obtained solid was filtered
3. customdried
4. dissolutiondissolved in 6 L of ethanol
5. additionThen, 840 g of thionyl chloride was added by drop for 2 hours
6. stirringstirred for 12 hours at 60° C
7. additionTo this mixture was added a solution of 1.22 kg of sodium bicarbonate in 15 L of water
8. filtrationthe produced solid was filtered
9. customdried