反応 #55094

反応方程式

hydroxylamine hydrochloride

sodium

ethyl α-naphthylcarbamoylacetate

hydroxylamine

→

α-Naphthylcarbamoylacetohydroxamic acid

収率 62.0%

溶媒

methanol

反応条件

後処理

1. 1
   その他After leaving the reactants in contact for 5 hours
2. 2
   その他the mixture is evaporated to dryness in vacuo
3. 3
   ろ過the solution is filtered over charcoal
4. 4
   その他the product is precipitated cold with 3 N HCl
5. 5
   ろ過filtered off
6. 6
   洗浄washed with water
7. 7
   その他CRL 40,518 is obtained by recrystallisation from ethanol

実験手順

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).

出典