5-Bromovanillin → 5-Bromo-3,4-dihydroxybenzaldehyde
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([O:11]C)[C:9]=1[OH:10])[CH:5]=[O:6].B(Br)(Br)Br>ClCCl>[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([OH:11])[C:9]=1[OH:10])[CH:5]=[O:6]参加物
4
実験手順
To a solution of 3-bromo-4-hydroxy-5-methoxybenzaldehyde (12.1 g, 0.52 mol) in dichloromethane (200 ml) was added 1.0 M boron tribromide in dichloromethane (2.2 eq, 115 ml) at 0°. The reaction was stirred at 0° for 20 min, then at ambient temperature for 2.5 h. The reaction was then cooled to 0°, and quenched by the slow addition of methanol. The solvents were removed under reduced pressure and the trimethyl borate was removed by azeotropation with added methanol. Drying in vacuo yielded the desired product (11.51 g, 100%).
後処理
- waitat ambient temperature for 2.5 h
- temperatureThe reaction was then cooled to 0°
- customquenched by the slow addition of methanol
- customThe solvents were removed under reduced pressure
- customthe trimethyl borate was removed by azeotropation with added methanol
- customDrying in vacuo
出典と根拠
- ORDレコード
- ord-822645d3364e415f8723a94d458026a1
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07732461B2
反応ノート
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