反応 #49918

ord-844de72b613a415f811a9289f1c17680

反応条件

温度
5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他from separate
  2. 2
    workup.ADDITIONaddition funnels
  3. 3
    温度while maintaining the temperature at or below 10° C
  4. 4
    workup.ADDITIONthe addition
  5. 5
    温度the reaction mixture was warmed to room temperature
  6. 6
    workup.ADDITIONThe reaction mixture was diluted with hexane

実験手順

To a stirred suspension of t-butylhydrazine hydrochloride (2 g, 0.016M) in toluene (50 ml) at room temperature was added dropwise a 50% aqueous solution of sodium hydroxide (1.28 g, 0.016M). After 15 minutes, the reaction mixture was cooled to 5° C. and a solution of benzoyl chloride (2.3 g, 0.017M) in toluene (5 ml) and a solution of aqueous 50% sodium hydroxide (1.36 g, 0.017M) were added dropwise simultaneously from separate addition funnels while maintaining the temperature at or below 10° C. Following the addition, the reaction mixture was warmed to room temperature and stirred for 1 hour. The reaction mixture was diluted with hexane and the solid N'-t-butyl-N-benzoylhydrazine was isolated by filtration.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05424333uspto-grants-1995_06