تفاعل #49913

ord-afd9ef446bce4af0b9c4f598804702b2

ظروف التفاعل

درجة الحرارة
5°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةsimultaneously so as to maintain the reaction temperature below 10° C
  2. 2
    workup.ADDITIONAfter the addition
  3. 3
    درجة الحرارةto warm to room temperature
  4. 4
    أخرىthe solid product isolated by filtration
  5. 5
    درجة الحرارةcooled on ice
  6. 6
    workup.STIRRINGwhile stirring
  7. 7
    workup.ADDITIONAfter addition
  8. 8
    workup.STIRRINGthe mixture was stirred for 1/2 hour

الإجراء التجريبي

To a stirred suspension of t-butylhydrazine hydrochloride (0.86 g, 0.007M) in toluene (30 ml) was added 50% sodium hydroxide (0.55 g, 0.007M). After 15 minutes, the mixture was cooled to 5° C. and cyclohexenylcarbonyl chloride (1.0 g, 0.007M) and 50% sodium hydroxide (0.55 g, 0.007M) were added separately and simultaneously so as to maintain the reaction temperature below 10° C. After the addition, the reaction mixture was allowed to warm to room temperature and stirred for 1 hour. The mixture was diluted with hexane and the solid product isolated by filtration. This product (1.2 g, 0.006M) was dissolved in toluene (30 ml) and cooled on ice while stirring. To this mixture was added benzoylchloride (1.0 g, 0.007M) and 50% sodium hydroxide (1.3 g, 0.007M) simultaneously. After addition, the mixture was stirred for 1/2 hour, diluted with hexane and the solid product, N'-t-butyl-N-cyclohexenylcarbonyl-N'-benzoylhydrazine, was isolated by filtration.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05424333uspto-grants-1995_06