반응식
[Br:1][C:2]1[C:7]([CH:8]=[O:9])=[C:6]([OH:10])[C:5]([O:11]C)=[CH:4][CH:3]=1.B(Br)(Br)Br>C(Cl)Cl>[Br:1][C:2]1[C:7]([CH:8]=[O:9])=[C:6]([OH:10])[C:5]([OH:11])=[CH:4][CH:3]=1참가 물질
4
반응 조건
- 온도
- 0 °C
실험 절차
6-Bromo-2-hydroxy-3-methoxybenzaldehyde (2.00 g, 8.65 mmol) was dissolved in methylene chloride (10 mL) and cooled to 0° C. Boron tribromide (17.0 mL of a 1.0 M solution, 17.00 mmol) was added by syringe and the solution was stirred at 0° C. for 1 h before allowing the reaction to warm up to ambient temperature and stir for 15 h at which time TLC analysis indicated the reaction complete. The reaction mixture was poured onto ice and extracted with ethyl acetate. The organic layers were dried with magnesium sulfate and concentrated by rotary evaporation to afford 1.82 g of 6-bromo-2,3-dihydroxybenzaldehyde (8.39 mmol, 97% yield) as a yellow solid.
후처리
- customthe reaction
- temperatureto warm up to ambient temperature
- stirringstir for 15 h at which time TLC analysis
- additionThe reaction mixture was poured onto ice
- extractionextracted with ethyl acetate
- dry with materialThe organic layers were dried with magnesium sulfate
- concentrationconcentrated by rotary evaporation
출처 및 근거
- ORD 기록
- ord-b4f0ffe745404e8e915ec68940ea06fe
- 출처 데이터셋
- uspto-grants-1999_09
- 특허 번호
- US05948817
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