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
Under nitrogen atmosphere, 3.7 g of 2-cyano-7-methoxynaphthalene was dissolved in 40 ml of dichloro- methane, and 6.6 ml of titanium tetrachloride and 4.6 ml of dichloromethyl methyl ether were added dropwise into the resulting solution at 0° in this order. The resulting mixture was stirred at room temperature for 30 minutes and cooled to 0° C. again. Water was added to the resulting mixture to cease the reaction, and the resulting mixture was extracted with dichloromethane (100 ml×2) The organic layers were combined, washed with water, a saturated aqueous solution of sodium bicarbonate and brine successively, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated and the resulting crude crystal was washed with ether and dried to give 3.3 g of the title compound as colorless crystals.
WORKUP
后处理
- temperaturecooled to 0° C. again
- customthe reaction
- extractionthe resulting mixture was extracted with dichloromethane (100 ml×2) The organic layers
- washwashed with water
- dry with materiala saturated aqueous solution of sodium bicarbonate and brine successively, dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationThe filtrate was concentrated
- washthe resulting crude crystal was washed with ether
- customdried