Reaktion #55094

Reaktionsgleichung

hydroxylamine hydrochloride

sodium

ethyl α-naphthylcarbamoylacetate

hydroxylamine

→

α-Naphthylcarbamoylacetohydroxamic acid

Ausbeute 62.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter leaving the reactants in contact for 5 hours
2. 2
   Sonstigethe mixture is evaporated to dryness in vacuo
3. 3
   Filtrationthe solution is filtered over charcoal
4. 4
   Sonstigethe product is precipitated cold with 3 N HCl
5. 5
   Filtrationfiltered off
6. 6
   Waschenwashed with water
7. 7
   SonstigeCRL 40,518 is obtained by recrystallisation from ethanol

Vorschrift

19.3 g (0.075 mol) of ethyl α-naphthylcarbamoylacetate are treated with a solution of hydroxylamine, prepared from 5.6 g (0.08 mol) of hydroxylamine hydrochloride and 3.68 g of sodium in 250 ml of methanol. After leaving the reactants in contact for 5 hours, the mixture is evaporated to dryness in vacuo, the residue is taken up in 400 ml of cold water, the solution is filtered over charcoal, and the product is precipitated cold with 3 N HCl, filtered off and washed with water. CRL 40,518 is obtained by recrystallisation from ethanol. Yield: 62%. Melting point: 184°-186° C. (with decomposition).

Quelle