3-Ethoxy-4-methylisoxazole-5-carboxylic acid → HCID 178431796、化合物
反応式
C([O:3][C:4]1[C:8]([CH3:9])=[C:7]([C:10]([OH:12])=[O:11])[O:6][N:5]=1)C>Br>[OH:3][C:4]1[C:8]([CH3:9])=[C:7]([C:10]([OH:12])=[O:11])[O:6][N:5]=1参加物
3
実験手順
3-Ethoxy-4-methylisoxazole-5-carboxylic acid (15 g, 88 mmol) and 47% HBr (aq) (150 mL) was boiled under reflux for 6 h. The solution was cooled and crystalline title compound was collected by filtration (8.7 g, 69%): mp 257-259° C. The acidic filtrate was added water (100 mL), and extracted with diethyl ether (6×400 mL). The organic extracts were washed with brine (100 mL), dried (MgSO4) and concentrated in vacuo to give crude title compound (3.0 g, 24%). Overall yield of 93%. A mixture of the two crops were used in the next step.
後処理
- temperatureunder reflux for 6 h
- temperatureThe solution was cooled
- filtrationcrystalline title compound was collected by filtration (8.7 g, 69%)
- additionThe acidic filtrate was added water (100 mL)
- extractionextracted with diethyl ether (6×400 mL)
- washThe organic extracts were washed with brine (100 mL)
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-16807d7db65f49948185baaab329c411
- 出典データセット
- uspto-grants-2001_03
- 特許番号
- US06200999B1
反応ノート
読み込み中…