反应详情

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.

1. temperatureThe reaction mixture was warmed to 60° C.
2. stirringstirred for 2 hours
3. extractionthe product extracted into methylene chloride (50 ml)
4. washThe methylene chloride layer was washed with water (5×20 ml)
5. dry with materialdried over anhydrous magnesium sulfate
6. customthe methylene chloride removed under vacuum