反应 #55094

ord-34e19f4dc75d49fc88b2096e844cd957

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04151300uspto-grants-1979_04