Hydroxyamine hydrochloride → Ethyl 5-cyclopropylisoxazole-4-carboxylate
反応式
Cl.[NH2:2]O.[CH:4]1([C:7](=[O:18])[C:8](=[CH:14]OCC)[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:6][CH2:5]1>CCO>[CH:4]1([C:7]2[O:18][N:2]=[CH:14][C:8]=2[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:6][CH2:5]1参加物
4
実験手順
A mixture of hydroxylamine hydrochloride (105.0 g, 1.51 mole), ethyl β-cyclopropyl-α-ethoxymethylene-β-ketopropionate (320.0 g, 1.51 mole) [prepared in Step A] and 1200 ml of EtOH was heated at reflux for 2 h. The solvent was removed in vacuo and the residue was partitioned between water and ether. The organic phase was separated, washed again with water, dried and evaporated to leave a dark, greasy solid. Trituration of the crude product under Skellysolve B gave 158 g of the title compound.
後処理
- temperaturewas heated
- temperatureat reflux for 2 h
- customThe solvent was removed in vacuo
- customthe residue was partitioned between water and ether
- customThe organic phase was separated
- washwashed again with water
- customdried
- customevaporated
- customto leave a dark, greasy solid
出典と根拠
- ORDレコード
- ord-b12de4bad36549e7b0205b25272885df
- 出典データセット
- uspto-grants-1990_06
- 特許番号
- US04935434
反応ノート
読み込み中…