Water → 6-Bromo-3,4-dimethoxybenzaldehyde

HRID 613029

反応式

HRID 613029 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH:6]=[O:7].[Br:13]Br.O>C(O)(=O)C>[Br:13][C:8]1[C:5]([CH:6]=[O:7])=[CH:4][C:3]([O:2][CH3:1])=[C:10]([O:11][CH3:12])[CH:9]=1

参加物

5

反応物 3

HCID 962WaterHCID 8419VeratraldehydeHCID 24408Bromine2 回

生成物 1

HCID 793516-Bromo-3,4-dimethoxybenzaldehyde

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

3,4-Dimethoxybenzaldehyde (398.8 g) is dissolved in acetic acid (1.8 liter), and thereto is added dropwise bromine (136 ml) at room temperature over a period of four hours. The mixture is stirred overnight, and thereto is added dropwise slowly again bromine (60 ml), and the mixture is stirred overnight. The reaction solution is added to water (7 liters), and the precipitated crystals are collected by filtration, washed with water, and dissolved in chloroform (2 liters). The chloroform solution is washed, dried, concentrated, and the residue is crystallized from diisopropyl ether to give 6-bromo-3,4-dimethoxybenzaldehyde (470 g) as a colorless crystal.

後処理

  1. stirringthe mixture is stirred overnight
  2. filtrationthe precipitated crystals are collected by filtration
  3. washwashed with water
  4. dissolutiondissolved in chloroform (2 liters)
  5. washThe chloroform solution is washed
  6. customdried
  7. concentrationconcentrated
  8. customthe residue is crystallized from diisopropyl ether

出典と根拠

ORDレコード
ord-16c7c1bee46443039c28bad0e39a7dec
出典データセット
uspto-grants-1999_12
特許番号
US06005106

関連ノート

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