HRID484968

反应详情

EQUATION

反应方程式

HRID 484968 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureis heated
  2. temperatureunder reflux for 1 hour
  3. customThe benzene is removed under reduced pressure
  4. dissolutionthe residual oil is dissolved in ethyl acetate
  5. customSSB (1:1) and chromatographed on silica gel
  6. washThe column is eluted with ethyl acetate
  7. concentrationconcentrated
  8. customthe product is crystallized from ethyl acetate