반응 #560173

ord-0b8e32ae7fa243aebe9cca9c6f902b45

시약

없음

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture was refluxed for 18 hours
  2. 2
    온도The mixture was cooled in ice bath
  3. 3
    기타removed the ice bath
  4. 4
    workup.ADDITIONadded water slowly
  5. 5
    여과The mixture was filtrated
  6. 6
    농축the filtrate was concentrated

실험 절차

A solution of phthalic acid (9 g, 0.05 mol) in anhydrous THF (200 mL) was added to LAH (7.6 g, 0.2 mol) in THF (250 mL) dropwise, and the mixture was refluxed for 18 hours. The mixture was cooled in ice bath and carefully added water dropwise, followed by 50% NaOH (150 mL), and then removed the ice bath added water slowly with stirring until the gray precipitate turns white. The mixture was filtrated and the filtrate was concentrated to give crude 1,2-phenylenedimethanol (7 g, 92%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08633212B2uspto-grants-2014_01