反応 #4854

ord-5155b74041e040c5848aa97537ebe3cb

溶媒

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the reaction mixture is cooled
  2. 2
    その他The precipitate formed
  3. 3
    その他then dried under vacuum
  4. 4
    その他is recrystallized from 170 ml of dioxane
  5. 5
    その他After being dried under vacuum

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04727192uspto-grants-1988_02