반응 #725852

ord-e686fe4dc07544349c8f09239672c13b

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added dropwise
  2. 2
    workup.ADDITIONAfter completion of the dropwise addition
  3. 3
    세척Thereafter, the organic layer was washed with water until it
  4. 4
    기타toluene was removed under reduced pressure
  5. 5
    기타The residue was recrystallized from n-hexane

실험 절차

To the same flask as used in Example 1 were added 340.51 g (1.0 mole) of 2,2'-methylenebis(6-tert-butyl-4-methylphenol), 86.41 g (1.0 mole) of 98.5% methacrylic acid, 500 g of toluene and 242.86 g (2.4 moles) of triethylamine. After replacing the air in the container with nitrogen, 229.14 g (1.2 moles) of o-toluenesulfonyl chloride was added dropwise with stirring. After completion of the dropwise addition, the reaction solution was kept at 90° 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 recrystallized from n-hexane to obtain 384.1 g of a white crystalline 2,2'-methylenebis(6-tert-butyl-4-methylphenol) monomethacrylate having a melting point of 144° to 146° C. Yield, 94%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04562281uspto-grants-1985_12