Sodium Hydroxide → 5-Bromo-4,6-dimethylpyridin-2-amine
反応式
[NH2:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[N:3]=1.[Br:10]Br.[OH-].[Na+]>C(O)(=O)C>[NH2:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([Br:10])=[C:4]([CH3:9])[N:3]=1参加物
5
実験手順
6.1 g (50 mmol) of 2-amino-4,6-dimethylpyridine are dissolved in 50 ml of acetic acid. A solution of 8 g (50 mmol) of bromine in 50 ml of acetic acid is added dropwise using a dropping funnel. The reaction medium is allowed to return to room temperature and the stirring is continued for 3 hours. The mixture is cooled in an ice bath and 40% sodium hydroxide is then added until the pH is basic. The mixture is filtered and dried. The residue is taken up in a little isopropyl ether and then chromatographed on silica gel, eluting with this same solvent. The expected product is collected in the form of white crystals. It is recrystallized from absolute ethanol.
後処理
- customto return to room temperature
- temperatureThe mixture is cooled in an ice bath
- filtrationThe mixture is filtered
- customdried
- customchromatographed on silica gel
- washeluting with this same solvent
- customThe expected product is collected in the form of white crystals
- customIt is recrystallized from absolute ethanol
出典と根拠
- ORDレコード
- ord-b746bfdddc774de5a31155dd8e6e752b
- 出典データセット
- uspto-grants-1998_01
- 特許番号
- US05712294
反応ノート
読み込み中…