Water → [1,1'-Biphenyl]-4,4'-dicarboxaldehyde

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.

1. additionTo this solution was added the reagent solution
2. customprepared above in drops at 5° C. or below
3. additionAfter the dropwise addition
4. customUpon completion of the reaction, extraction
5. concentrationwas concentrated until dryness under reduced pressure
6. dissolutionThe residue was dissolved in acetone
7. additionby adding 303.2 g of acetone in drops
8. addition1600.3 g of water was added in drops at 20° C
9. stirringThereafter, the mixture was stirred day and night at 5° C.
10. filtrationa solid was recovered by filtration
11. customThe solid thus obtained
12. washwas washed with acetone
13. customdried under reduced pressure

ORDレコード

ord-25c872cf8d544280ace618887109e235

出典データセット

uspto-grants-2009_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07582364B2