Water → 7-Bromo-1,3-dioxaindane-5-carbaldehyde
反応式
[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]=1参加物
6
反応条件
- 温度
- 140 °C
実験手順
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
後処理
- 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
出典と根拠
- ORDレコード
- ord-0d38999cde49444faa0534a1045bfd1b
- 出典データセット
- uspto-grants-2007_03
- 特許番号
- US07196108B2
反応ノート
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