反応 #49907

反応方程式

HCl

allyl iodide

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

sodium hydride

→

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

溶媒

water

DMF

反応条件

後処理

1. 1
   温度The reaction mixture was warmed to 60° C.
2. 2
   workup.STIRRINGstirred for 2 hours
3. 3
   抽出the product extracted into methylene chloride (50 ml)
4. 4
   洗浄The methylene chloride layer was washed with water (5×20 ml)
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   その他the methylene chloride removed under vacuum

実験手順

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.

出典