Sodium Bicarbonate → HCID 67468970, Verbindung

HRID 1890810

Reaktionsgleichung

Reaktionsgleichung von HRID 1890810
Cl.[F:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][NH2:10].Cl.N[C:13]([O:20]CC)=[CH:14][C:15]([O:17][CH2:18][CH3:19])=O.C(=O)(O)[O-].[Na+]>C(O)C>[CH2:18]([O:17][C:15]1[CH2:14][C:13](=[O:20])[N:9]([C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=2[F:2])[N:10]=1)[CH3:19]

Komponenten

5

Edukt 3

HCID 516892Sodium BicarbonateHCID 2723910Hydrazine, (2-fluorophenyl)-, hydrochloride (1:1)HCID 53395434Ethyl beta-amino-beta-ethoxyacrylate hydrochloride

Produkt 1

HCID 67468970HCID 67468970, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

(2-Fluorophenyl)hydrazine hydrochloride (1.00 g, 6.15 mmol) was suspended in ethanol (10 mL), treated with ethyl 3-amino-3-ethoxyacrylate hydrochloride (1.20 g, 6.15 mmol, 1.00 equiv), and placed into a preheated oil bath at 70° C. for 5 hours. The mixture was cooled to ambient temperature, poured into saturated aqueous sodium bicarbonate (100 mL), and extracted with ethyl acetate (3×75 mL). The combined organic extracts were dried with sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by silica gel chromatography (100:0 to 0:100 hexanes:ethyl acetate), providing the titled compound.

Aufarbeitung

  1. extractionextracted with ethyl acetate (3×75 mL)
  2. dry with materialThe combined organic extracts were dried with sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by silica gel chromatography (100:0 to 0:100 hexanes:ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-39dd79331e9a4fb28dcd15ed78f95851
Quelldatensatz
uspto-grants-2013_08
Patentnummer
US08507494B2

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