반응 #338896

ord-662ab2c2ce3042cdaf44c23f1b91f5dc

용매

반응 조건

온도
155°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling the mixture to room temperature
  2. 2
    workup.STIRRINGagitated at 80° C. for ten minutes
  3. 3
    여과Solid precipitate was collected by filtration
  4. 4
    세척washed with 7 L of ion-exchange water
  5. 5
    기타dried under reduced pressure

실험 절차

In a 5 L recovery flask, 48.4 g of 3,3′-dibromo-5,5′,7,7′-tetramethyl-1,1′-biadamantane (100 mmol), 688 g of phenol (7.3 mol) and a stirrer were charged and agitated at 155° C. for 30 minutes under nitrogen flow. After cooling the mixture to room temperature, 4.3 L of ion-exchange water was added thereto and agitated at 80° C. for ten minutes. Solid precipitate was collected by filtration, then washed with 7 L of ion-exchange water and dried under reduced pressure, thus obtaining 50.6 g of 3,3′-bis(4-hydroxyphenyl)-5,5′,7,7′-tetramethyl-1,1′-biadamantane (99.0 mmol; yield: 99.0%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07863347B2uspto-grants-2011_01