Hydrogen Bromide → 2,3-Dihydroxybenzaldehyde

HRID 37546

반응식

HRID 37546 반응식
[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]

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 8991o-Vanillin

생성물 1

HCID 905792,3-Dihydroxybenzaldehyde수율 70.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-8e7891df21cc4ed39de4bc1a4c84a2c9
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420308

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