반응 #68035

ord-3a1e10de7d8d4e789b490a43f855051d

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    온도under cooling with ice
  3. 3
    추출the resultant solution was extracted with ethyl acetate
  4. 4
    세척The organic layer was washed with an aqueous saturated sodium chloride solution
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    기타the solvent was removed under reduced pressure

실험 절차

To 30 mL of a tetrahydrofuran solution containing 1.06 g of methyl 8-methoxy-2,3-dihydro-1,4-benzodioxin-6-carboxylate, 720 mg of lithium aluminum hydride was added under cooling with ice. The reaction mixture was stirred at room temperature for 1 hour, 5 mL of a 1 mol/L hydrochloric acid and 45 mL of water were added thereto, and the resultant solution was extracted with ethyl acetate. The organic layer was washed with an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to obtain 940 mg of a brown oily substance, (8-methoxy-2,3-dihydro-1,4-benzodioxin-6-yl)methanol.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08524738B2uspto-grants-2013_09