Reaktion #1500903

Reaktionsgleichung

Sodium hydride

4-(phenylmethyl)piperazinone

mehyl iodide

→

title compound

1-Methyl-4-(phenylmethyl)piperazinone

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe reaction solution is refluxed for 2.5 hours
2. 2
   SonstigeThe THF is removed under reduced pressure
3. 3
   Sonstigethe residual oil is partitioned between chloroform and water
4. 4
   SonstigeEvaporation of the chloroform
5. 5
   Sonstigegives an oil which
6. 6
   Sonstigeis chromatographed on silica gel

Vorschrift

Sodium hydride (50% in oil, 10.4 g., 0.22 mole) is added to a stirred solution of 4-(phenylmethyl)piperazinone (Example 45, 38.0 g., 0.20 mole) in THF (2.0 l.). After 1 hour mehyl iodide (80.0 g., 0.75 mole) is added and the reaction solution is refluxed for 2.5 hours. The THF is removed under reduced pressure and the residual oil is partitioned between chloroform and water. Evaporation of the chloroform gives an oil which is chromatographed on silica gel to give the title compound, which is converted to the p-TSA salt, m.p. 138°-140°.

Quelle