반응 #812501
ord-3c8aae4684b94cbf887056e9a2e6acc0
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도heated
- 2온도under reflux
- 3workup.ADDITIONare added
- 4여과the separated precipitate is filtered under suction
- 5세척washed with water
- 6여과filtered over 50 g of aluminum oxide (activity grade The crystalline material
- 7기타obtained
- 8기타is 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°.