تفاعل #55094

ord-34e19f4dc75d49fc88b2096e844cd957

معادلة التفاعل

Cl.NO
hydroxylamine hydrochloride
[Na]
sodium
CCOC(=O)CC(=O)Nc1cccc2ccccc12
ethyl α-naphthylcarbamoylacetate
NO
hydroxylamine
O=C(CC(=O)Nc1cccc2ccccc12)NO
α-Naphthylcarbamoylacetohydroxamic acid
المردود 62.0%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter leaving the reactants in contact for 5 hours
  2. 2
    أخرىthe mixture is evaporated to dryness in vacuo
  3. 3
    ترشيحthe solution is filtered over charcoal
  4. 4
    أخرىthe product is precipitated cold with 3 N HCl
  5. 5
    ترشيحfiltered off
  6. 6
    غسيلwashed with water
  7. 7
    أخرىCRL 40,518 is obtained by recrystallisation from ethanol

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04151300uspto-grants-1979_04