反应详情

To the mixture of 8.9 g of 2-amino-5-dimethylaminobenzoic acid in 60 mL of dioxane, under stirring and external cold water cooling 10 mL of diphosgene is added dropwise. The mixture is heated under reflux conditions for 4 hours. From the cold reaction mixture the solid material is filtered off, washed with 50 mL of ether. The product is stirred for 5 minutes in the mixture of 50 mL of methanol and 5 mL of triethylamine, filtered off, washed with 30 mL of methanol. After drying 7 g of the title product is obtained, m.p.: 258° C.

1. temperatureThe mixture is heated under reflux conditions for 4 hours
2. customFrom the cold reaction mixture the solid material
3. filtrationis filtered off
4. washwashed with 50 mL of ether
5. stirringThe product is stirred for 5 minutes in the mixture of 50 mL of methanol and 5 mL of triethylamine
6. filtrationfiltered off
7. washwashed with 30 mL of methanol
8. dry with materialAfter drying 7 g of the title product
9. customis obtained