Sulfuric Acid → HCID 18950694, Verbindung

HRID 1492552Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1492552
O1CCOCC1.CO.C([NH:11][CH:12]([C:25]1[CH:26]=[N:27][CH:28]=[CH:29][CH:30]=1)[CH2:13][CH2:14][C:15]1[CH:24]=[CH:23][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:17][CH:16]=1)=O.S(=O)(=O)(O)O.C(=O)([O-])O.[Na+]>>[NH2:11][CH:12]([C:25]1[CH:26]=[N:27][CH:28]=[CH:29][CH:30]=1)[CH2:13][CH2:14][C:15]1[CH:24]=[CH:23][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:17][CH:16]=1

Komponenten

4

Edukt 3

HCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 86748334HCID 86748334, Verbindung

Produkt 1

HCID 18950694HCID 18950694, VerbindungAusbeute 87,4 %

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To 10 ml of the solution of 0.62 g of methyl 4-[3-formamido-3-(3-pyridyl)propyl]benzoate methanol-1,4 dioxane (1:1) was added 5 ml of 4% sulfuric acid, and stirred under heating at 60° C. overnight, which was then poured into saturated aqueous sodium hydrogencarbonate solution to be extracted with ethyl acetate. The obtained ethyl acetate phase was washed in saturated aqueous sodium chloride and dried over magnesium sulfate, to distill off the solvent, so that 0.35 g of methyl 4-[3-amino-3-(3-pyridyl)propyl]benzoate was yielded.

Aufarbeitung

  1. extractionto be extracted with ethyl acetate
  2. washThe obtained ethyl acetate phase was washed in saturated aqueous sodium chloride
  3. dry with materialdried over magnesium sulfate
  4. distillationto distill off the solvent

Quellen und Nachweise

ORD-Eintrag
ord-f3c8f0436cd3406f85d86598960cc551
Quelldatensatz
uspto-grants-1994_12
Patentnummer
US05374641

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