HRID371422
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 50 ml of anhydrous pyridine, was added 2.4 g of 2-methylbenzoic acid followed by 4.4 g of DCC under cooling in ice. After stirring for 30 minute and adding 5.0 g of 6-amidino-2-naphthol methanesulfonate, the mixture was stirred overnight at room temperature. The precipitate was collected by filtration and washed with a small volume of pyridine, then successively with ethylether and acetone. The precipitate was dissolved in DMF and the insolubles were removed by filtration. Ethylether was added to the filtrate and the precipitated crystals were recrystallized from ethanol to obtain 1.4 g of flaky colorless crystals of 6-amidino-2-naphthyl 2-methyl benzoate methanesulfonate.
WORKUP
后处理
- temperatureunder cooling in ice
- stirringthe mixture was stirred overnight at room temperature
- filtrationThe precipitate was collected by filtration
- washwashed with a small volume of pyridine
- dissolutionThe precipitate was dissolved in DMF
- customthe insolubles were removed by filtration
- additionEthylether was added to the filtrate
- customthe precipitated crystals were recrystallized from ethanol