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
12.1 g of sodium hydride and 580 mL of 1,2-dimethoxyethane were placed in a three-neck flask, and while stirring at room temperature, 108.5 g of tetramethyl phosphonium bromide was added. After adding one drop of anhydrous ethanol, the mixture was reacted for 4 hours at 70° C. 100 g of 4-[N,N-bis-(3,4-dimethylphenyl) amino] benzaldehyde was added to the reaction mixture, and the mixture was reacted for 5 hours at 70° C. The reaction solution was filtered, and an ether extract of the filtered cake and filtrate were washed in water. The ether solution was dehydrated with calcium chloride. The ether was removed and the reaction mixture was obtained. This was recrystallized twice with ethanol, and a needle-form of 4-[N,N-bis-(3,4-dimethylphenyl) amino] styrene was obtained. The amount obtained was 84.5 g (yield rate of 85.0%).
WORKUP
后处理
- customthe mixture was reacted for 4 hours at 70° C
- customthe mixture was reacted for 5 hours at 70° C
- filtrationThe reaction solution was filtered
- extractionan ether extract of the filtered cake and filtrate
- washwere washed in water
- customThe ether was removed
- customthe reaction mixture was obtained
- customThis was recrystallized twice with ethanol