反应详情

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.

1. temperaturewas heated
2. temperatureat reflux for 2 h
3. customThe solvent was removed in vacuo
4. customthe residue was partitioned between water and ether
5. customThe organic phase was separated
6. washwashed again with water
7. customdried
8. customevaporated
9. customto leave a dark, greasy solid