反応 #49897

反応方程式

benzoyl chloride

sodium hydroxide

sodium hydroxide

t-butylhydrazine hydrochloride

→

N'-t-butyl-N,N'-dibenzoylhydrazine

溶媒

toluene

toluene

反応条件

後処理

1. 1
   その他simultaneously from separate
2. 2
   workup.ADDITIONaddition funnels
3. 3
   温度while maintaining the temperature 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 ether
7. 7
   その他the product isolated by filtration
8. 8
   洗浄The product was washed with water and ether
9. 9
   その他dried
10. 10
    その他The product was recrystallized from ether-methanol

実験手順

To a stirred suspension of t-butylhydrazine hydrochloride (1.24 g, 10 mmoles) in toluene (50 ml) at room temperature, was added dropwise a solution of 50% aqueous sodium hydroxide (0.8 g, 10 ml). After 15 minutes, the reaction mixture was cooled to 5° C. and solutions of benzoyl chloride (2.82 gm, 20 ml) in toluene (7 ml) and 50% aqueous sodium hydroxide (1.6 g) were added dropwise and simultaneously from separate addition funnels while maintaining the temperature below 10° C. Following the addition, the reaction mixture was warmed to room temperature and stirred for 1 hr. The reaction mixture was diluted with ether and the product isolated by filtration. The product was washed with water and ether and dried. The product was recrystallized from ether-methanol to afford N'-t-butyl-N,N'-dibenzoylhydrazine as a white powder: m.p. 174°-176° C.

出典