HRID1172311
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of benzyl 3-oxo-2,3-dihydrospiro[indene-1,4′-piperidine]-1′-carboxylate (3 g, 10.3 mmol) in EtOH (30 mL) containing NH2OH.HCl (1.43 g, 20.6 mmol) and NaOAc (1.52 g, 18.53 mmol) was heated under reflux for 1.5 h. The solvent was removed by evaporation and the residue was partitioned between CH2Cl2 and water. The organic phase was washed with brine, dried over Na2SO4, and concentrated to provide benzyl 3-(hydroxyimino)-2,3-dihydrospiro[indene-1,4′-piperidine]-1′-carboxylate (3.14 g, yield 99%), which was used directly in the next step.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 1.5 h
- customThe solvent was removed by evaporation
- customthe residue was partitioned between CH2Cl2 and water
- washThe organic phase was washed with brine
- dry with materialdried over Na2SO4
- concentrationconcentrated