반응 #725856

반응 방정식

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

acryloyl chloride

hydrochloric acid

→

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

수율 94.7%

용매

triethylamine

toluene

triethylamine

반응 조건

후처리

1. 1
   기타To a 500-ml 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
   workup.STIRRINGstirring
6. 6
   기타the formed triethylamine hydrochloride was then removed
7. 7
   세척by washing with water
8. 8
   기타Toluene was then removed by evaporation from the toluene layer after completion of the washing
9. 9
   기타the residue obtained
10. 10
    기타was recrystallized from 20 g of n-hexane

실험 절차

To a 500-ml four-necked flask equipped with a thermometer, stirring apparatus, condenser and dropping funnel were added 82.0 g (0.241 mole) of 2,2'-methylenebis(6-tert-butyl-4-methylphenol), 200 g of toluene and 23.9 g (0.290 mole) of triethylamine. After replacing the air in the container with nitrogen, 25 g (0.276 mole) of acryloyl chloride was added dropwise with stirring. After completion of the dropwise addition, stirring was continued for 1 hour, excess triethylamine was neutralized with a dilute hydrochloric acid and the formed triethylamine hydrochloride was then removed by washing with water. Toluene was then removed by evaporation from the toluene layer after completion of the washing, and the residue obtained was recrystallized from 20 g of n-hexane to obtain 90.0 g of 2,2'-methylenebis(6-tert-butyl-4-methylphenol) monoacrylate as a white crystal. Melting point, 132°-134° C. Yield, 95%.

출처