반응 #4854

ord-5155b74041e040c5848aa97537ebe3cb

용매

반응 조건

온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the reaction mixture is cooled
  2. 2
    기타The precipitate formed
  3. 3
    기타then dried under vacuum
  4. 4
    기타is recrystallized from 170 ml of dioxane
  5. 5
    기타After being dried under vacuum

실험 절차

0.39 Mole (88 g) of 2,3-dihydro-5,7-dinitro-2-methylbenzofuran, prepared according to J.A.C.S. 80, p. 4711-4714 (1958), is suspended in 1.1 l of 20% strength ammonia solution and 600 ml of Methyl Cellosolve. After 18 hours' heating at 70° C., the reaction mixture is cooled. The precipitate formed is drained and, after being made into a paste in water until neutral and then dried under vacuum, is recrystallized from 170 ml of dioxane. After being dried under vacuum, 0.30 mole (72 g) of the expected product is obtained; it melts at 177° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04727192uspto-grants-1988_02