Hydroxyamine hydrochloride → Ethyl 5-cyclopropylisoxazole-4-carboxylate
반응식
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]1참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-b12de4bad36549e7b0205b25272885df
- 출처 데이터셋
- uspto-grants-1990_06
- 특허 번호
- US04935434
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