反応 #2328977

反応方程式

water

THF

potassium-t-butoxide

methoxymethyltriphenylphosphonium chloride

THF

bicyclohexyl-4,4′-dione

→

white solid

4,4′-bis(methoxymethylidene)bicyclohexyl

反応条件

後処理

1. 1
   温度while maintaining the inner temperature
2. 2
   workup.ADDITIONadded dropwise
3. 3
   workup.STIRRINGAfter stirring for 1 hour
4. 4
   workup.ADDITIONwas added
5. 5
   その他thereby terminating
6. 6
   その他the 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
    ろ過further filtration (twice)
12. 12
    洗浄washed in turn with an aqueous 50% methanol solution and saturated saline
13. 13
    乾燥dried over anhydrous magnesium sulfate
14. 14
    workup.DISTILLATIONThe solvent was distilled off

実験手順

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.

出典