Reaktion #572150

Reaktionsgleichung

1-(phenylmethyl)piperazinone

1-(Phenylmethyl)piperazinone hydrochloride

2-(t-butoxycarbonyloxyimino)-2-phenylacetamide

→

title compound

4-(t-Butoxycarbonyl)-1-(phenylmethyl)piperazinone

Lösungsmittel

benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturis heated
2. 2
   Temperaturunder reflux for 1 hour
3. 3
   SonstigeThe benzene is removed under reduced pressure
4. 4
   workup.DISSOLUTIONthe residual oil is dissolved in ethyl acetate
5. 5
   SonstigeSSB (1:1) and chromatographed on silica gel
6. 6
   WaschenThe column is eluted with ethyl acetate
7. 7
   Einengenconcentrated
8. 8
   Sonstigethe product is crystallized from ethyl acetate

Vorschrift

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°.

Quelle