反应详情

To the mixture of 8.9 g of 2-amino-5-(2,6-dimethylmorpholin-4-yl)benzoic 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, then filtered off and washed with 30 ml of methanol. After drying 7 g of the title product is obtained (MH+: 277).

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 (MH+: 277)