HRID484968
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 mixture of 1-(phenylmethyl)piperazinone (XIV, Example 40, 19.0 g., 0.1 mole) and 2-(t-butoxycarbonyloxyimino)-2-phenylacetamide (30.0 g., 0.12 mole) in benzene (200 ml.) is heated under reflux for 1 hour. The benzene is removed under reduced pressure, the residual oil is dissolved in ethyl acetate:SSB (1:1) and chromatographed on silica gel. The column is eluted with ethyl acetate, the appropriate fractions are pooled, concentrated and the product is crystallized from ethyl acetate:SSB (1:10) to give the title compound, m.p. 89°-90°.
WORKUP
后处理
- temperatureis heated
- temperatureunder reflux for 1 hour
- customThe benzene is removed under reduced pressure
- dissolutionthe residual oil is dissolved in ethyl acetate
- customSSB (1:1) and chromatographed on silica gel
- washThe column is eluted with ethyl acetate
- concentrationconcentrated
- customthe product is crystallized from ethyl acetate