反应 #2340888

ord-9c9e7d789a524600963e2e266ac32313

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度under reflux for 2 hours
  3. 3
    温度the whole mixture was heated
  4. 4
    温度under reflux for a further 30 minutes
  5. 5
    温度After the mixture had been cooled
  6. 6
    其他to precipitate crystals
  7. 7
    过滤These crystals were collected by filtration
  8. 8
    其他recrystallized from ethanol

实验过程

A mixture of 2.5 g of 2-(4-t-butoxycarbonylaminophenyl)-3-oxobutyronitrile, 20 ml of ethanol and 1.4 g of 2,2-diethoxyethylhydrazine was heated under reflux for 2 hours. 20 ml of 4N hydrogen chloride in dioxane were added, and then the whole mixture was heated under reflux for a further 30 minutes. After the mixture had been cooled, ethyl acetate was added to precipitate crystals. These crystals were collected by filtration and recrystallized from ethanol to give 1.4 g of the title compound as pale brown plates melting at 180°-190° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05232939uspto-grants-1993_08