Reaktion #49907

Reaktionsgleichung

HCl

allyl iodide

N'-t-butyl-N,N'-dibenzoylhydrazine

sodium hydride

→

N-allyl-N'-t-butyl-N,N'-dibenzoylhydrazine

Lösungsmittel

water

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was warmed to 60° C.
2. 2
   workup.STIRRINGstirred for 2 hours
3. 3
   Extraktionthe product extracted into methylene chloride (50 ml)
4. 4
   WaschenThe methylene chloride layer was washed with water (5×20 ml)
5. 5
   Trocknendried over anhydrous magnesium sulfate
6. 6
   Sonstigethe methylene chloride removed under vacuum

Vorschrift

To a stirred solution of N'-t-butyl-N,N'-dibenzoylhydrazine (3 g, 0.011M) in DMF (30 ml) at room temperature under nitrogen was added portionwise sodium hydride (60% oil dispersion) (0.5 g, 0.012M). The mixture was stirred at room temperature for 0.5 hours, and then allyl iodide (1.8 g, 0.01M) was added dropwise. The reaction mixture was warmed to 60° C. and stirred for 2 hours. The mixture was then diluted with water (50 ml), neutralized with 10% HCl and the product extracted into methylene chloride (50 ml). The methylene chloride layer was washed with water (5×20 ml), dried over anhydrous magnesium sulfate and the methylene chloride removed under vacuum to afford N-allyl-N'-t-butyl-N,N'-dibenzoylhydrazine as an oil.

Quelle