반응 #816397

반응 방정식

water

dimethyl 4,4′-biphenyldicarboxylate

THF

→

4,4′-biphenyldicarboxaldehyde

수율 86.1%

용매

methylene chloride

methylene chloride

반응 조건

후처리

1. 1
   workup.ADDITIONTo this solution was added the reagent solution
2. 2
   기타prepared above in drops at 5° C. or below
3. 3
   workup.ADDITIONAfter the dropwise addition
4. 4
   기타Upon completion of the reaction, extraction
5. 5
   농축was concentrated until dryness under reduced pressure
6. 6
   workup.DISSOLUTIONThe residue was dissolved in acetone
7. 7
   workup.ADDITIONby adding 303.2 g of acetone in drops
8. 8
   workup.ADDITION1600.3 g of water was added in drops at 20° C
9. 9
   workup.STIRRINGThereafter, the mixture was stirred day and night at 5° C.
10. 10
    여과a solid was recovered by filtration
11. 11
    기타The solid thus obtained
12. 12
    세척was washed with acetone
13. 13
    기타dried under reduced pressure

실험 절차

Next, 27.1 g (0.10 mole) of dimethyl 4,4′-biphenyldicarboxylate and 133.4 g of THF were introduced to a 2000-ml four-necked reaction vessel. To this solution was added the reagent solution prepared above in drops at 5° C. or below. After the dropwise addition, stirring was continued at 15° C. for 4.5 hours. Upon completion of the reaction, extraction was performed by adding in drops 622.2 g of methylene chloride and 411.2 g of water. The methylene chloride layer obtained was concentrated until dryness under reduced pressure. The residue was dissolved in acetone by adding 303.2 g of acetone in drops and then 1600.3 g of water was added in drops at 20° C. Thereafter, the mixture was stirred day and night at 5° C. and a solid was recovered by filtration. The solid thus obtained was washed with acetone and dried under reduced pressure to give 18.1 g of 4,4′-biphenyldicarboxaldehyde.

출처