반응 #725850

반응 방정식

phosphorus oxychloride

2,2'-methylenebis(6-tert-butyl-4-methylphenol)

acrylic acid

triethylamine

→

2,2'-methylenebis(6-tert-butyl-4-methylphenol) monoacrylate

수율 95.0%

용매

toluene

반응 조건

후처리

1. 1
   기타To a 2-liter four-necked flask equipped with a thermometer
2. 2
   workup.ADDITIONwas added dropwise
3. 3
   workup.STIRRINGwith stirring
4. 4
   workup.ADDITIONAfter completion of the dropwise addition
5. 5
   세척Thereafter, the organic layer was washed with water until it
6. 6
   기타toluene was removed under reduced pressure
7. 7
   기타The residue was then recrystallized from n-hexane

실험 절차

To a 2-liter four-necked flask equipped with a thermometer, stirring apparatus, condenser and dropping funnel were added 340.51 g (1.0 mole) of 2,2'-methylenebis(6-tert-butyl-4-methylphenol), 72.06 g (1.0 mole) of acrylic acid, 500 g of toluene and 209.47 g (2.07 moles) of triethylamine. After replacing the air in the container with nitrogen, 105.8 g (0.69 mole) of phosphorus oxychloride was added dropwise with stirring. After completion of the dropwise addition, the reaction solution was kept at 80° C. for 1 hour. Thereafter, the organic layer was washed with water until it became neutral, and toluene was removed under reduced pressure. The residue was then recrystallized from n-hexane to obtain 374.8 g of a white crystalline 2,2'-methylenebis(6-tert-butyl-4-methylphenol) monoacrylate having a melting point of 132° to 134° C. Yield, 95%.

출처