Hydrogen Bromide → 2,3-Dihydroxybenzaldehyde

HRID 37546

反応式

HRID 37546 の反応式
[O:1]=[CH:2][C:3]1[CH:11]=[CH:10][CH:9]=[C:6]([O:7]C)[C:4]=1[OH:5].Br>C(O)(=O)C>[OH:5][C:4]1[C:6]([OH:7])=[CH:9][CH:10]=[CH:11][C:3]=1[CH:2]=[O:1]

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 8991o-Vanillin

生成物 1

HCID 905792,3-Dihydroxybenzaldehyde収率 70.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

152.0 g (1.0 mol) of o-vanillin and 200 ml of azeotropic hydrobromic acid (47.5% strength) are stirred under reflux in 500 ml of glacial acetic acid for 2.5 hours. The acid mixture is then distilled off and the residue is subjected to fractional vacuum distillation. The redistilled fraction having a boiling point of 120°-125° C./12 mbar is purified by recrystallisation from 1 l of heptane (hexane is also possible and is recovered). 97 g (70% of theory) of 2,3-dihydroxybenzaldehyde of melting point 105°-107° C. are obtained.

後処理

  1. distillationThe acid mixture is then distilled off
  2. distillationthe residue is subjected to fractional vacuum distillation
  3. customis purified by recrystallisation from 1 l of heptane (hexane
  4. customis recovered)

出典と根拠

ORDレコード
ord-8e7891df21cc4ed39de4bc1a4c84a2c9
出典データセット
uspto-grants-1995_05
特許番号
US05420308

関連ノート

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