Water → HCID 178488949, Verbindung

HRID 745437

Reaktionsgleichung

Reaktionsgleichung von HRID 745437
[C:1](OCC)(=[O:6])[CH2:2][C:3]([CH3:5])=O.[CH3:10][O:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([NH2:18])=[NH:17])=[CH:14][CH:13]=1.O>C(Cl)(Cl)Cl>[OH:6][C:1]1[N:18]=[C:16]([C:15]2[CH:19]=[CH:20][C:12]([O:11][CH3:10])=[CH:13][CH:14]=2)[N:17]=[C:3]([CH3:5])[CH:2]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 8868Ethyl AcetoacetateHCID 2290744-Methoxybenzenecarboximidamide

Produkt 1

HCID 178488949HCID 178488949, VerbindungAusbeute 75 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

Under N2, a solution of ethyl acetoacetate (7.15 g, 0.053 mol) in CHCl3 (200 ml) was added dropwise to a suspension of 4-methoxybenzamidine in CHCl3 (200 ml). After stirring at room temperature overnight, water was added to the solution. The aqueous phase was separated and extracted with CHCl3 and the organic layers were combined, dried (Na2SO4), filtered and concentrated to dryness. The residue was chromatographed on silica gel and the product was eluted with 2% CH3OH--CHCl3 to yield 8.58 g (75%) of product, m.p. 198°-199° C.

Aufarbeitung

  1. customThe aqueous phase was separated
  2. extractionextracted with CHCl3
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated to dryness
  6. customThe residue was chromatographed on silica gel
  7. washthe product was eluted with 2% CH3OH

Quellen und Nachweise

ORD-Eintrag
ord-e992968ba96e4ce48b7d3fea3bb6058d
Quelldatensatz
uspto-grants-1986_07
Patentnummer
US04598149

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