Hydroxyamine hydrochloride → HCID 86736790, Verbindung

HRID 2052403Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2052403
[Na].Cl.[NH2:3][OH:4].[CH3:5][O:6][C:7]1[CH:8]=[C:9]([NH:17][C:18]([CH2:20][C:21](OCC)=[O:22])=[O:19])[CH:10]=[C:11]([O:15][CH3:16])[C:12]=1[O:13][CH3:14]>CO>[CH3:5][O:6][C:7]1[CH:8]=[C:9]([OH:4])[CH:10]=[C:11]([O:15][CH3:16])[C:12]=1[O:13][CH3:14].[C:18]([CH2:20][C:21]([NH:3][OH:4])=[O:22])(=[O:19])[NH2:17]

Komponenten

5

Edukt 3

HCID 443297Hydroxyamine hydrochlorideHCID 5360545SodiumHCID 54077321Ethyl 3,4,5-trimethoxyphenylcarbamoylacetate

Produkt 1

HCID 86736790HCID 86736790, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

4.15 g (0.18 gram atom) of sodium are added in small pieces to 100 ml of anhydrous methanol and this cold solution is then poured into a solution of 7 g (0.1 mol) of hydroxylamine hydrochloride in 100 ml of methanol; the sodium chloride is filtered off and 23.8 g (0.08 mol) of ethyl 3,4,5-trimethoxyphenylcarbamoylacetate are added to the filtrate. The reactants are left in contact overnight, the mixture is evaporated to dryness in vacuo, the residue is taken up in water, the solution is acidified with 3 N HCl and the product is filtered off and washed with cold water and with diisopropyl ether. recrystallisation from methanol gives CRL 40,509. Melting point=195°-196° C. (with decomposition).

Aufarbeitung

  1. filtrationthe sodium chloride is filtered off
  2. customthe mixture is evaporated to dryness in vacuo
  3. filtrationthe product is filtered off
  4. washwashed with cold water and with diisopropyl ether
  5. customrecrystallisation from methanol
  6. customgives CRL 40,509

Quellen und Nachweise

ORD-Eintrag
ord-760bd40f43a84ba19089f0af03b233bf
Quelldatensatz
uspto-grants-1980_01
Patentnummer
US04183951

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