반응식
[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]=1참가 물질
5
실험 절차
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.
후처리
- stirringthe mixture is stirred overnight
- filtrationthe precipitated crystals are collected by filtration
- washwashed with water
- dissolutiondissolved in chloroform (2 liters)
- washThe chloroform solution is washed
- customdried
- concentrationconcentrated
- customthe residue is crystallized from diisopropyl ether
출처 및 근거
- ORD 기록
- ord-16c7c1bee46443039c28bad0e39a7dec
- 출처 데이터셋
- uspto-grants-1999_12
- 특허 번호
- US06005106
연결된 노트
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