반응 #812501

ord-3c8aae4684b94cbf887056e9a2e6acc0

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated
  2. 2
    온도under reflux
  3. 3
    workup.ADDITIONare added
  4. 4
    여과the separated precipitate is filtered under suction
  5. 5
    세척washed with water
  6. 6
    여과filtered over 50 g of aluminum oxide (activity grade The crystalline material
  7. 7
    기타obtained
  8. 8
    기타is recrystallized from ethyl acetate/n-hexane

실험 절차

5.0 g of 4-hydroxy-5-methoxy-isophthalaldehyde are treated with 50 ml of constant-boiling hydrobromic acid and heated to boiling under reflux and while stirring under an argon atmosphere for 3 hours. After cooling 50 ml of ice-water are added thereto, and the separated precipitate is filtered under suction and washed with water. The crude product is taken up in ethyl acetate and filtered over 50 g of aluminum oxide (activity grade The crystalline material obtained is recrystallized from ethyl acetate/n-hexane. There is obtained 4,5-dihydroxyisophthalaldehyde in the form of slightly orange crystals of m.p. 201°-202°.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05705703uspto-grants-1998_01