Реакция #49907

ord-1f565d8e745b4d0f90d3eefa8cd0e70b

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe reaction mixture was warmed to 60° C.
  2. 2
    workup.STIRRINGstirred for 2 hours
  3. 3
    Экстракцияthe product extracted into methylene chloride (50 ml)
  4. 4
    ПромывкаThe methylene chloride layer was washed with water (5×20 ml)
  5. 5
    Сушкаdried over anhydrous magnesium sulfate
  6. 6
    Другоеthe methylene chloride removed under vacuum

Методика

To a stirred solution of N'-t-butyl-N,N'-dibenzoylhydrazine (3 g, 0.011M) in DMF (30 ml) at room temperature under nitrogen was added portionwise sodium hydride (60% oil dispersion) (0.5 g, 0.012M). The mixture was stirred at room temperature for 0.5 hours, and then allyl iodide (1.8 g, 0.01M) was added dropwise. The reaction mixture was warmed to 60° C. and stirred for 2 hours. The mixture was then diluted with water (50 ml), neutralized with 10% HCl and the product extracted into methylene chloride (50 ml). The methylene chloride layer was washed with water (5×20 ml), dried over anhydrous magnesium sulfate and the methylene chloride removed under vacuum to afford N-allyl-N'-t-butyl-N,N'-dibenzoylhydrazine as an oil.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05424333uspto-grants-1995_06