반응 #568172

ord-c745c41559344da384c7120717f66ec7

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONA three neck round bottom flask containing a teflon coated magnetic stirring bar
  2. 2
    기타An addition funnel, thermometer, and a short path still head with thermometer and receiver flask were placed in the flask necks
  3. 3
    기타The flask was placed in an oil bath
  4. 4
    온도the temperature was increased until distillation
  5. 5
    workup.ADDITIONwas added dropwise at the same rate as the distillate
  6. 6
    온도The reaction mixture was heated for 4 hours
  7. 7
    workup.DISTILLATIONdistilled

실험 절차

A three neck round bottom flask containing a teflon coated magnetic stirring bar was successively charged with 95 mL (0.884 mol) of methyl methacrylate (2), 4.22 g (0.012 mol) of titanium tetrabutoxide (Ti(OC4H9)4), 50 mL (0.316 mol) of 3-benzyloxy-1-propanol (1), and 14.6 g (0.073 mol) of 4-benzyloxyphenol (4-BOP). An addition funnel, thermometer, and a short path still head with thermometer and receiver flask were placed in the flask necks. The flask was placed in an oil bath and the temperature was increased until distillation began. Methyl methacrylate (2) was placed in the addition funnel and was added dropwise at the same rate as the distillate. The reaction mixture was heated for 4 hours and then cooled to room temperature. The crude product was vacuum distilled to isolate 36.5 g (0.156 mol, 49%) of 3-benzyloxypropyl methacrylate (3) as a clear, colorless liquid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06653422B2uspto-grants-2003_11