반응 #6984

ord-c6cbca41f26745508b2a75aeede61ad4

용매

반응 조건

온도
90°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타prepared
  2. 2
    온도After cooling
  3. 3
    기타to exceed 5° C
  4. 4
    기타the precipitate obtained
  5. 5
    여과is filtered off
  6. 6
    세척washed with cold water

실험 절차

A mixture of 2.50 g (0.011 mmol) of methyl-3-(methoxycarbonyl)amino-4-methoxy-isoxazole-5-carboxylate (prepared according to the method described in W. Kloetzer, J. Schantz, Monatsh. Chem., 1965, 102–115) and 1.30 g of powdered sodium hydroxide dissolved in 9 ml of water is heated at 90° C. for 3 hours. After cooling, the mixture is acidified to pH=2 with concentrated hydrochloric acid, controlling the temperature so as not to exceed 5° C. After 1 hour of stirring at 0° C., the precipitate obtained is filtered off and washed with cold water. There is obtained 2.01 g (86% yield) of a white solid (M+1=217).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07084163B2uspto-grants-2006_08