Reaktion #1822202

Reaktionsgleichung

4-bromobenzoic hydrazide

1-bromo-2-fluoroethane

sodium hydroxide

→

oil

Ausbeute 64.1%

2-(4-Bromophenyl)-4H-1,3,4-Oxadiazine

Ausbeute 64.1%

Lösungsmittel

ethanol

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe resulting solution was refluxed for two and one-half hours
2. 2
   Extraktionextracted several times with ether (100 ml)
3. 3
   SonstigeAfter separation
4. 4
   Trocknendrying over anhydrous sodium sulfate
5. 5
   Filtrationthe solution was filtered
6. 6
   Sonstigeevaporated under reduced pressure

Vorschrift

A solution of 2.9 g (0.07 mole) sodium hydroxide dissolved in 10 ml of water was added dropwise at room temperature to a mixture of 6.5 g (0.03 mole) 4-bromobenzoic hydrazide and 4.0 g (0.03 mole) 1-bromo-2-fluoroethane in 25 ml of ethanol. The resulting solution was refluxed for two and one-half hours. The mixture was cooled to room temperature, diluted with 150 ml of water and extracted several times with ether (100 ml). After separation and drying over anhydrous sodium sulfate, the solution was filtered and evaporated under reduced pressure leaving 4.6 grams of an oil (63.6% yield), which was purified by distillation. The product was characterized by IR and NMR spectroscopy.

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