Reaktion #2328977

Reaktionsgleichung

water

THF

potassium-t-butoxide

methoxymethyltriphenylphosphonium chloride

THF

bicyclohexyl-4,4′-dione

→

white solid

4,4′-bis(methoxymethylidene)bicyclohexyl

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwhile maintaining the inner temperature
2. 2
   workup.ADDITIONadded dropwise
3. 3
   workup.STIRRINGAfter stirring for 1 hour
4. 4
   workup.ADDITIONwas added
5. 5
   Sonstigethereby terminating
6. 6
   Sonstigethe reaction
7. 7
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure and hexane
8. 8
   workup.ADDITIONwas added
9. 9
   workup.STIRRINGby stirring
10. 10
    workup.STIRRINGvigorous stirring
11. 11
    Filtrationfurther filtration (twice)
12. 12
    Waschenwashed in turn with an aqueous 50% methanol solution and saturated saline
13. 13
    Trocknendried over anhydrous magnesium sulfate
14. 14
    workup.DISTILLATIONThe solvent was distilled off

Vorschrift

882.3 g of methoxymethyltriphenylphosphonium chloride was dispersed in 2,600 mL of THF, followed by cooling to −10° C. 313.2 g of potassium-t-butoxide were added while maintaining the inner temperature. After stirring or one hours, a THF (800 mL) solution of 200.0 g of bicyclohexyl-4,4′-dione was and added dropwise. After stirring for 1 hour while maintaining the inner temperature, water was added thereby terminating the reaction. The solvent was distilled off under reduced pressure and hexane was added, followed by stirring and vigorous stirring and further filtration (twice). The filtrates were combined, washed in turn with an aqueous 50% methanol solution and saturated saline, and then dried over anhydrous magnesium sulfate. The solvent was distilled off to obtain 231.8 g of a white solid.

Quelle