Hydrogen Bromide → 2-Amino-5-chloro-3-hydroxybenzoic acid
반응식
[NH2:1][C:2]1[C:10]([O:11]C)=[CH:9][C:8]([Cl:13])=[CH:7][C:3]=1[C:4]([O-:6])=[O:5].Br.C([O-])([O-])=O.[Na+].[Na+]>C(O)(=O)C>[NH2:1][C:2]1[C:10]([OH:11])=[CH:9][C:8]([Cl:13])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]참가 물질
5
실험 절차
A mixture of 2-amino-5-chloro-3-methoxybenzoate (2.76 g, 12.8 mmol), 48% aqueous solution of hydrobromic acid (25 mL) and glacial acetic acid (1 mL) was heated to reflux for 48 h. The reaction mixture was cooled down to room temperature, treated with saturated solution of Na2CO3 to pH6, concentrated and purified by column chromatography (silica gel, 90:10 dichloromethane/methano 1) to afford 2-amino-5-chloro-3-hydroxybenzoic acid (0.84 g, 35%) as a light brown solid: MS (ESI+) m/z 188 (M+H).
후처리
- temperaturewas heated
- temperatureto reflux for 48 h
- concentrationconcentrated
- custompurified by column chromatography (silica gel, 90:10 dichloromethane/methano 1)
출처 및 근거
- ORD 기록
- ord-89305917de044695b53917fb43d919ed
- 출처 데이터셋
- uspto-grants-2010_08
- 특허 번호
- US07781430B2
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