Reaktion #2465331

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
   workup.ADDITIONcontaining
2. 2
   Sonstige<0.5% of di- and poly-brominated compounds and prepared as per the method
3. 3
   Sonstigeof 30 minutes
4. 4
   Sonstigeat −20° C. to −5° C
5. 5
   TemperaturThe temperature was raised to 5 to 10° C.
6. 6
   Sonstigethe reaction mixture purged with nitrogen gas for one to two hours
7. 7
   workup.ADDITIONThe solution containing 4-bromo-2-methoxyimino-3-oxo butyric acid chloride (IV)
8. 8
   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. 97%; containing <0.5% of di- and poly-brominated compounds and prepared as per the method disclosed in WO 03/045899) 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