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Water → HCID 22013867, Verbindung

HRID 1532740
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1532740
[H-].[Na+].[H][H].C1(C)C=CC(S([O:14][CH2:15][CH2:16][C:17]2[N:18]=[C:19]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[O:20][C:21]=2[CH3:22])(=O)=O)=CC=1.[OH2:30].[C:31]([O:34][CH2:35][CH3:36])(=[O:33])[CH3:32]>CCCCCC.CN(C)C=O>[C:17]([NH:18][CH:32]([CH2:19][C:23]1[CH:28]=[CH:27][C:26]([O:14][CH2:15][CH2:16][C:17]2[N:18]=[C:19]([C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=3)[O:20][C:21]=2[CH3:22])=[CH:25][CH:24]=1)[C:31]([O:34][CH2:35][CH3:36])=[O:33])(=[O:30])[CH3:16]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 962WaterHCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 120517392-(5-Methyl-2-phenyloxazol-4-yl)ethyl 4-methylbenzenesulfonateHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 22013867HCID 22013867, VerbindungAusbeute 37 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittel2×HCID 8058HexaneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

Sodium hydride (60% in oil, 440 mg, 11.0 mmol) was washed twice with n-hexane (5 ml) under a nitrogen atmosphere, and suspended in N,N-dimethylformamide (50 ml) and ice-cooled. To this suspension was added ethyl N-acetyl-L-tyrosine ester (2.51 g, 10.0 mmol) over 15 min. Ten minutes later when hydrogen bubbling ended, a solution of 2-(5-methyl-2-phenyl-4-oxazolyl)ethyl p-toluenesulfonate (3.57 g, 10.0 mmol) in N,N-dimethylformamide (50 ml) was added. The mixture was stirred at 80° C. for 3 hr, and water (50 ml) and ethyl acetate (100 ml×2) were added for partition. The obtained organic layer was washed with saturated brine (100 ml), dried over magnesium sulfate and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (developing solvent; dichloromethane:methanol=98:2) to give the title compound (1.63 g, yield 37%) as a white solid.

Aufarbeitung

  1. temperatureice-cooled
  2. customfor partition
  3. washThe obtained organic layer was washed with saturated brine (100 ml)
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe obtained residue was purified by silica gel column chromatography (developing solvent; dichloromethane:methanol=98:2)

Quellen und Nachweise

ORD-Eintrag
ord-ab95d491c880408ab9b1fc146f1b27d2
Quelldatensatz
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06204277B1

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