HRID373518
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 19.4 g of 2,3,4,6-tetrafluorobenzoic acid, 200 ml of dioxane and 35.3 ml of benzylamine was heated under reflux for 3 hours. The reaction mixture was concentrated to dryness under reduced pressure. Water was added to the residue, and hydrochloric acid was added to adjust the pH of the solution to 3. The solution was then extracted with ethyl acetate. The extract was dried, treated with activated carbon and concentrated. Ether and n-hexane were added to the residue, and the crystals were collected by filtration to give 20.2 g of 2-benzylamino-3,4,6-trifluorobenzoic acid. m.p. 140-141° C.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 3 hours
- concentrationThe reaction mixture was concentrated to dryness under reduced pressure
- additionWater was added to the residue, and hydrochloric acid
- additionwas added
- extractionThe solution was then extracted with ethyl acetate
- customThe extract was dried
- additiontreated with activated carbon
- concentrationconcentrated
- additionEther and n-hexane were added to the residue
- filtrationthe crystals were collected by filtration