Hydrochloric Acid → 6-Amino-5-iodo-2-(methyloxy)-3-pyridinecarboxylic acid
反応式
[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[C:5]([C:10]([O:12]C)=[O:11])=[CH:4][C:3]=1[I:14].[OH-].[Li+].Cl>CO.O>[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[C:5]([C:10]([OH:12])=[O:11])=[CH:4][C:3]=1[I:14]参加物
6
反応条件
- 温度
- 70 °C
実験手順
To a solution of methyl 6-amino-5-iodo-2-(methyloxy)-3-pyridinecarboxylate (1.4 g, 4.54 mmol) in methanol (30 ml), 1M aqueous lithium hydroxide (9 ml, 9 mmol) was added and the mixture was heated at 70° C. for 2 h. After cooling to room temperature, the mixture was concentrated in vacuo to give a solid. The residual solid was dissolved in water (50 ml) and acidified (pH=5) by addition of 2N aqueous hydrochloric acid. The resultant solid was collected by filtration, washed with water and dried in vacuo under 60° C. to give 1.3 g (92%) of the title compound.
後処理
- temperatureAfter cooling to room temperature
- concentrationthe mixture was concentrated in vacuo
- customto give a solid
- filtrationThe resultant solid was collected by filtration
- washwashed with water
- customdried in vacuo under 60° C.
出典と根拠
- ORDレコード
- ord-356adbb358054d1b8c63afb83e93b00f
- 出典データセット
- uspto-grants-2005_12
- 特許番号
- US06979690B2
反応ノート
読み込み中…