Water → 7-Bromo-1,3-dioxaindane-5-carbaldehyde
반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([OH:11])[C:9]=1[OH:10])[CH:5]=[O:6].[F-].[K+].Br[CH2:15]Br.O>CN(C=O)C>[Br:1][C:2]1[C:9]2[O:10][CH2:15][O:11][C:8]=2[CH:7]=[C:4]([CH:5]=[O:6])[CH:3]=1참가 물질
6
반응 조건
- 온도
- 140 °C
실험 절차
To a solution of 3-bromo-4,5-dihydroxy-benzaldehyde (1.52 g, 7.02 mmol) in DMF (20 mL), were added KF (4.077 g, 70.18 mmol) followed by dibromomethane (1 mL, 14.04 mmol) and the mixture heated at 140° C. for 4 hours. The solution was cooled to room temperature, water was added and the mixture extracted with ether. The organic layer was further washed with saturated aqueous NaHCO3, dried (MgSO4), filtered and evaporated to give 973 mg of 7-bromo-benzo[1,3]dioxole-5-carbaldehyde. 1H NMR (300 MHz; CDCl3): δ 6.16 (s, 2H), 7.26 (s, 1H), 7.54 (s, 1H), 9.76
후처리
- temperatureThe solution was cooled to room temperature
- extractionthe mixture extracted with ether
- washThe organic layer was further washed with saturated aqueous NaHCO3
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated
출처 및 근거
- ORD 기록
- ord-0d38999cde49444faa0534a1045bfd1b
- 출처 데이터셋
- uspto-grants-2007_03
- 특허 번호
- US07196108B2
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