Hydrochloric Acid → 6-Chloro-3-methylimidazo[1,2-a]pyridine-2-carboxylic acid
反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8]([CH3:15])=[C:9]([C:11]([O:13]C)=[O:12])[N:10]=2)[CH:7]=1.[OH-].[K+].Cl>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8]([CH3:15])=[C:9]([C:11]([OH:13])=[O:12])[N:10]=2)[CH:7]=1参加物
5
反応条件
- 温度
- 50 °C
実験手順
To a solution of methyl 6-chloro-3-methylimidazo[1,2-a]pyridine-2-carboxylate (1.01 g, 4.50 mmol) in MeOH (18 mL) at room temperature was added potassium hydroxide (407 mg, 7.25 mmol). The reaction mixture was heated to 50° C. for 15 h, and additional KOH (293 mg) was added. The reaction mixture was heated to reflux for 1 h, cooled to room temperature and 5 M HCl (2.5 mL) was added and the reaction mixture was concentrated. toluene (25 mL) was added to the concentrate and the toluene was evaporated under reduced pressure. This was repeated a second time and the concentrate was dried under high vacuum to give 6-chloro-3-methylimidazo[1,2-a]pyridine-2-carboxylic acid as an off white solid. MS m/z=210.9 [M+H]
後処理
- temperatureThe reaction mixture was heated
- temperatureto reflux for 1 h
- temperaturecooled to room temperature
- concentrationthe reaction mixture was concentrated
- additiontoluene (25 mL) was added to the
- concentrationconcentrate
- customthe toluene was evaporated under reduced pressure
- customthe concentrate was dried under high vacuum
出典と根拠
- ORDレコード
- ord-bb286cd4472249ec8b3f3a0975508911
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09309263B2
反応ノート
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