반응 #55094

반응 방정식

hydroxylamine hydrochloride

sodium

ethyl α-naphthylcarbamoylacetate

hydroxylamine

→

α-Naphthylcarbamoylacetohydroxamic acid

수율 62.0%

용매

methanol

반응 조건

후처리

1. 1
   기타After leaving the reactants in contact for 5 hours
2. 2
   기타the mixture is evaporated to dryness in vacuo
3. 3
   여과the solution is filtered over charcoal
4. 4
   기타the product is precipitated cold with 3 N HCl
5. 5
   여과filtered off
6. 6
   세척washed with water
7. 7
   기타CRL 40,518 is obtained by recrystallisation from ethanol

실험 절차

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).

출처