反应 #2994

反应方程式

sodium chloride

3-nitro-4-methylbenzaldehyde

3,4,5-trimethoxybenzyltriphenylphosphine bromide

sodium hydride

→

intended compound

收率 49.6%

(Z)-1-(3-nitro-4-methylphenyl)-2-(3,4,5-trimethoxyphenyl)ethene

收率 49.6%

溶剂

benzene

benzene

acetic acid

反应条件

后处理

1. 1
   workup.ADDITIONdispersed
2. 2
   workup.ADDITIONtherein was added
3. 3
   其他reacted for 15 hours at room temperature
4. 4
   其他The reaction liquid
5. 5
   workup.ADDITIONwas added
6. 6
   萃取the resulting liquid was extracted with dichloromethane
7. 7
   干燥The extract was dried with anhydrous sodium sulfate
8. 8
   浓缩concentrated
9. 9
   其他purified by silica gel column chromatography (diethyl ether:hexane=1:2 by volume)

实验过程

1.0 g of 3-nitro-4-methylbenzaldehyde and 3.3 g of 3,4,5-trimethoxybenzyltriphenylphosphine bromide were dissolved in 50 ml of benzene, and a benzene solution containing 302 mg of sodium hydride dispersed therein was added thereto and reacted for 15 hours at room temperature. The reaction liquid was neutralized with acetic acid, saturated sodium chloride solution was added thereto, and the resulting liquid was extracted with dichloromethane. The extract was dried with anhydrous sodium sulfate, concentrated and then purified by silica gel column chromatography (diethyl ether:hexane=1:2 by volume) to obtain 0.99 g of the intended compound. The yield of the product was 47.8%.

来源