Hydrogen Bromide → 2-Amino-5-chloro-3-hydroxybenzoic acid
反応式
[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]参加物
5
実験手順
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 pH˜6, concentrated and purified by column chromatography (silica gel, 90:10 dichloromethane/methanol) 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).
後処理
- temperaturewas heated
- temperatureto reflux for 48 h
- concentrationconcentrated
- custompurified by column chromatography (silica gel, 90:10 dichloromethane/methanol)
出典と根拠
- ORDレコード
- ord-0e5be3ed41ca4c0da3856d870bf48f1c
- 出典データセット
- uspto-grants-2007_12
- 特許番号
- US07307094B2
反応ノート
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