HRID1985662
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To the mixture of 8.9 g of 2-amino-5-(morpholin-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, it is filtered off and washed with 30 mL of methanol. After drying 7 g of the title product is obtained, m.p.: 235° C.
WORKUP
后处理
- temperatureThe mixture is heated under reflux conditions for 4 hours
- customFrom the cold reaction mixture the solid material
- filtrationis filtered off
- washwashed with 50 mL of ether
- stirringThe product is stirred for 5 minutes in the mixture of 50 mL of methanol and 5 mL of triethylamine, it
- filtrationis filtered off
- washwashed with 30 mL of methanol
- dry with materialAfter drying 7 g of the title product
- customis obtained