반응 #2994

반응 방정식

sodium chloride

3-nitro-4-methylbenzaldehyde

3,4,5-trimethoxybenzyltriphenylphosphine bromide

sodium hydride

→

intended compound

수율 49.6%

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

수율 49.6%

용매

benzene

benzene

acetic acid

반응 조건

후처리

1. 1
   workup.ADDITIONdispersed
2. 2
   workup.ADDITIONtherein was added
3. 3
   기타reacted for 15 hours at room temperature
4. 4
   기타The reaction liquid
5. 5
   workup.ADDITIONwas added
6. 6
   추출the resulting liquid was extracted with dichloromethane
7. 7
   건조The extract was dried with anhydrous sodium sulfate
8. 8
   농축concentrated
9. 9
   기타purified by silica gel column chromatography (diethyl ether:hexane=1:2 by volume)

실험 절차

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%.

출처