Hydrochloric Acid → HCID 15012465, compound

Temperature

-20 °C

Under a nitrogen atmosphere, 430 mg (2 mmol) of diphenyl carbonate and 5 mL of 2-butanone were loaded into a round bottom flask having a volume of 100 mL, and then the mixture was stirred at −20° C. A solution prepared by dissolving 550 mg (2 mmol) of 1-ethyl-3-methylimidazolium phenylalanine salt in 15 mL of 2-butanone was slowly dropped to the solution, and then the mixture was stirred at −20° C. for 8 hours. After that, a 1M aqueous HCl solution was added to the mixture to terminate the reaction. The resultant was concentrated with an evaporator. Next, water was added to the concentrated product, and then the resultant was extracted with ethyl acetate. After that, the resultant was concentrated with an evaporator. Thus, a crude product was obtained. Next, the crude product was purified by column chromatography. Thus, N-phenoxycarbonyl-L-phenylalanine was obtained. An isolation amount and an isolation yield were 528.9 mg and 93%, respectively.

1. customA solution prepared
2. additionwas slowly dropped to the solution
3. stirringthe mixture was stirred at −20° C. for 8 hours
4. customto terminate
5. customthe reaction
6. concentrationThe resultant was concentrated with an evaporator
7. additionNext, water was added to the concentrated product
8. extractionthe resultant was extracted with ethyl acetate
9. concentrationAfter that, the resultant was concentrated with an evaporator
10. customThus, a crude product was obtained
11. customNext, the crude product was purified by column chromatography

ORD record

ord-a8d2b34dc2eb449ba25330556850dc0d

Source dataset

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08748650B2