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Potassium Iodide → Phenylalanine,N-acetyl--phenyl-

HRID 32863
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 32863
[C:1]([NH:4][CH:5](C(OCC)=O)[C:6]([O:8]CC)=[O:7])(=[O:3])[CH3:2].[H-].[Na+].[C:18]1([C:24](Cl)(Cl)[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.[I-].[K+]>CN1CCCC1=O.O.C1(C)C=CC=CC=1>[C:1]([NH:4][CH:5]([CH:24]([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:6]([OH:8])=[O:7])(=[O:3])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 4875Potassium IodideHCID 14041Acetamidomalonic acid diethyl esterHCID 16327DichlorodiphenylmethaneHCID 24758Sodium hydride

Produkt 1

HCID 11022400Phenylalanine,N-acetyl--phenyl-Ausbeute 70,6 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962
Water
Lösungsmittel
HCID 1140TolueneLösungsmittel
HCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Versuchsvorschrift

To a solution (1.25 M) of diethyl acetamidomalonate (6.79 g, 31.25 mmol) in N-methyl-2-pyrrolidone (25 mL) was added 60% sodium hydride (1.25 g, 31.25 mmol), and the mixture was stirred at room temperature for 1 hr. Diphenylmethylene chloride (4.45 mL, 25.0 mmol) and potassium iodide (4.15 g, 25 mmol) were added, and the mixture was stirred at 50° C. for 7 hrs. After completion of the reaction, toluene (75 mL) and water (31.5 mL) were added to the reaction mixture, and the mixture was partitioned. The organic layer was washed twice with water (31.5 mL) and concentrated. Ethanol (31.5 mL) and 2M aqueous sodium hydroxide solution (37.5 mL) were added to the concentrated solution, and the mixture was stirred at 80° C. for 11 hrs and allowed to cool to 25° C. Toluene (9 mL) was added and the mixture was partitioned. The aqueous layer was concentrated to a half volume and adjusted to pH 1.1 with concentrated hydrochloric acid, which resulted in the precipitation of white crystals. The crystals were collected by filtration and dried under vacuum to give the title compound (5.0 g).

Aufarbeitung

  1. stirringthe mixture was stirred at 50° C. for 7 hrs
  2. additionwere added to the reaction mixture
  3. customthe mixture was partitioned
  4. washThe organic layer was washed twice with water (31.5 mL)
  5. concentrationconcentrated
  6. additionEthanol (31.5 mL) and 2M aqueous sodium hydroxide solution (37.5 mL) were added to the concentrated solution
  7. stirringthe mixture was stirred at 80° C. for 11 hrs
  8. temperatureto cool to 25° C
  9. additionToluene (9 mL) was added
  10. customthe mixture was partitioned
  11. concentrationThe aqueous layer was concentrated to a half volume
  12. customresulted in the precipitation of white crystals
  13. filtrationThe crystals were collected by filtration
  14. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-7318754b6aba48fd88690eb8de09f9e7
Quelldatensatz
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07427688B2

Notizen zur Reaktion

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