반응 #1592498

ord-5bfc12b90ce54a438f0fdd5a44317135

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The catalyst was filtered off
  2. 2
    workup.ADDITIONthe solution was diluted with a saturated solution of Na2CO3 (10 mL)
  3. 3
    추출extracted with ethyl acetate (2 times 60 mL)
  4. 4
    건조Combined organic layers were dried over sodium sulphate
  5. 5
    여과filtered
  6. 6
    기타evaporated to the title compound (1.25 g) as a brown/red solid

실험 절차

To a solution of 1-methyl-2-(methyloxy)-4-[(4-nitrophenyl)oxy]benzene (Intermediate 19, 1.43 g) in tetrahydrofuran (65 mL)/water (32.5 mL) iron (1.540 g, 27.6 mmol) and then ammonium chloride (1.475 g, 27.6 mmol) were added and the reaction mixture was stirred for 5 hours at room temperature. The catalyst was filtered off and the solution was diluted with a saturated solution of Na2CO3 (10 mL) and extracted with ethyl acetate (2 times 60 mL). Combined organic layers were dried over sodium sulphate, filtered and evaporated to the title compound (1.25 g) as a brown/red solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09216967B2uspto-grants-2015_12