Sulfamic Acid → 5-Fluoro-2-methoxynicotinic acid
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:10]=[O:11])[C:5]([O:8][CH3:9])=[N:6][CH:7]=1.Cl([O-])=[O:13].[Na+].O1CCOCC1.S(=O)(=O)(O)N>O>[F:1][C:2]1[CH:7]=[N:6][C:5]([O:8][CH3:9])=[C:4]([CH:3]=1)[C:10]([OH:13])=[O:11]参加物
6
実験手順
In a round bottom flask, 5-fluoro-2-methoxy-pyridine-3-carbaldehyde (37, 0.500 g, 3.22 mmol) was combined with sodium chlorite (0.6734 g, 5.957 mmol), 30 mL of 1,4-dioxane, 10 mL of water, and sulfamic acid (2.39 g, 24.6 mmol). The reaction mixture was stirred at room temperature for 5 minutes, then poured into 100 mL of water and extracted with 100 mL of ethyl acetate. The organic layer was washed with water, brine, then dried over magnesium sulfate, filtered and the filtrate concentrated under vacuum to provide the desired compound (150, 512 mg), used in the next step without further purification.
後処理
- extractionextracted with 100 mL of ethyl acetate
- washThe organic layer was washed with water, brine
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationthe filtrate concentrated under vacuum
出典と根拠
- ORDレコード
- ord-bbee6f56fd694b78920c04558da802e4
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09096593B2
反応ノート
読み込み中…