Reaktion #49910

Reaktionsgleichung

benzoylchloride

sodium hydroxide

sodium hydroxide

cyclohexanecarbonylchloride

sodium hydroxide

t-butylhydrazine hydrochloride

→

N'-t-butyl-N-cyclohexylcarbonyl-N'-benzoylhydrazine

Lösungsmittel

hexane

toluene

hexane

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperatursimultaneously so as to maintain the reaction temperature below 10° C
2. 2
   workup.ADDITIONAfter the addition
3. 3
   Temperaturto warm to room temperature
4. 4
   Sonstigethe solid product isolated by filtration
5. 5
   Temperaturcooled on ice
6. 6
   workup.ADDITIONAfter addition
7. 7
   workup.STIRRINGthe mixture was stirred for 1/2 hour

Vorschrift

To a stirred suspension of t-butylhydrazine hydrochloride (2.0 g, 0.016M) in toluene (30 ml) was added 50% sodium hydroxide (1.3 g, 0.016M). After 15 minutes, the mixture was cooled to 5° C. and cyclohexanecarbonylchloride (2.4 g, 0.016M) and 50% sodium hydroxide (1.3 g, 0.016M) 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 (1.5 g, 0.008M) was dissolved in a stirred mixture of toluene (30 ml) and cooled on ice. To this mixture was added benzoylchloride (1.1 g, 0.008M) and 50% sodium hydroxide (0.6 g, 0.008M) simultaneously. After addition, the mixture was stirred for 1/2 hour, diluted with hexane and the solid product, N'-t-butyl-N-cyclohexylcarbonyl-N'-benzoylhydrazine, isolated by filtration.

Quelle