Reaktion #2465332

Reaktionsgleichung

phosphorous pentachloride

4-bromo-2-methoxyimino-3-oxo butyric acid

→

4-bromo-2-methoxyimino-3-oxo butyric acid chloride

Lösungsmittel

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe temperature was raised to 5 to 10° C.
2. 2
   Sonstigethe reaction mixture purged with nitrogen gas for one to two hours
3. 3
   workup.ADDITIONThe solution containing 4-bromo-2-methoxyimino-3-oxo butyric acid chloride (IV)
4. 4
   Temperaturwas cooled to −10° C.

Vorschrift

To a suspension of phosphorous pentachloride (64.91 gm; 0.3113 moles) in dichloromethane (250 ml), cooled to −20° C. was added a solution of 4-bromo-2-methoxyimino-3-oxo butyric acid (66.41 gm; 0.2965 moles; purity ca. 87%; containing 4-5% of di- and poly-brominated compounds) in dichloromethane (250 ml) over a period of 30 minutes at −20° C. to -5° C. The temperature was raised to 5 to 10° C. and the reaction mixture purged with nitrogen gas for one to two hours to expel out hydrogen chloride gas. The solution containing 4-bromo-2-methoxyimino-3-oxo butyric acid chloride (IV) was cooled to −10° C.

Quelle