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 18 g of 6-amidino-2-naphthyl 5-aminomethylfuran-2-carboxylate dihydrochloride in 380 ml of DMF was added 19.1 ml of pyridine and then, while cooling with ice, 20 ml of a benzene solution containing 7.5 ml of 3-methoxycarbonylpropionyl chloride was added dropwise thereto for 20 minutes. After stirring at room temperature for 2.5 hours, the reaction mixture was added to 2 l of ether while stirring and cooling with ice, and the mixture was stirred at the same temperature for 5 hours. The supernatant was decanted and 1.5 l of ether was further added and stirred at room temperature for 18 hours. The precipitate was collected by filtration, 800 ml of acetone was added thereto, the mixture was stirred at room temperature for 5 hours, and the crystals were collected by filtration to obtain 19.6 g of the intended product.
WORKUP
后处理
- additionwas added dropwise
- stirringwhile stirring
- temperaturecooling with ice
- stirringthe mixture was stirred at the same temperature for 5 hours
- customThe supernatant was decanted
- addition1.5 l of ether was further added
- stirringstirred at room temperature for 18 hours
- filtrationThe precipitate was collected by filtration, 800 ml of acetone
- additionwas added
- stirringthe mixture was stirred at room temperature for 5 hours
- filtrationthe crystals were collected by filtration