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
To a solution of 11.6 g of 4-guanidinobenzoic acid hydrochloride in 180 ml of dried pyridine, while being cooled in ice, was added 13.2 g of DCC. After 30 minutes of stirring, 18.0 g of 4-amidino-2-benzoylphenol methanesulfonate was added, and the mixture was further stirred overnight at room temperature. A white solid substance precipitated from the reaction mixture was collected by filtration, washed with acetone, and dissolved in water. The aqueous solution was freed from the water-insoluble DCU by filtration and added to a saturated aqueous sodium bicarbonate solution, while being cooled in ice and stirred. The precipitated pale yellow crystals were collected by filtration, washed with water, then with acetone, and dried to yield 4-amidino-2-benzoylphenyl 4-guanidinobenzoate carbonate.
WORKUP
后处理
- waitthe mixture was further stirred overnight at room temperature
- customA white solid substance precipitated from the reaction mixture
- filtrationwas collected by filtration
- washwashed with acetone
- dissolutiondissolved in water
- filtrationThe aqueous solution was freed from the water-insoluble DCU by filtration
- additionadded to a saturated aqueous sodium bicarbonate solution
- temperaturewhile being cooled in ice
- stirringstirred
- filtrationThe precipitated pale yellow crystals were collected by filtration
- washwashed with water
- dry with materialwith acetone, and dried