HRID638674

反应详情

EQUATION

反应方程式

HRID 638674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

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%.

WORKUP

后处理

  1. customTo a 500-ml four-necked flask equipped with a thermometer
  2. additionwas added dropwise
  3. stirringwith stirring
  4. additionAfter completion of the dropwise addition
  5. stirringstirring
  6. customthe formed triethylamine hydrochloride was then removed
  7. washby washing with water
  8. customToluene was then removed by evaporation from the toluene layer after completion of the washing
  9. customthe residue obtained
  10. customwas recrystallized from 20 g of n-hexane