反应详情

温度

23 °C

A solution of N'-t-butyl-N-benzoylhydrazine (2.0 g) and nicotinoyl chloride hydrochloride in 20 ml of methylene chloride at 23° C. was treated dropwise with triethylamine (4 ml). The reaction mixture was stirred at 23° C. for 0.5 hours. Solids were removed by filtration. The filtrate was diluted with N/10 HCl and ether. The layers were separated and the organic layer was washed with N/10 HCl. The aqueous layer was neutralized with solid sodium bicarbonate and extracted with ether. The ether extracts were treated with charcoal and then dried with magnesium sulfate. Evaporation of solvents afforded a yellow oil which was chromatographed on silica gel using 10% CH3OH, 40% CH2Cl2, 50% Et2O as eluant to afford N'-t-butyl-N-benzoyl-N'-nicotinoylhydrazine as a yellow foam. m.p. 60°-63° C.

1. customSolids were removed by filtration
2. additionThe filtrate was diluted with N/10 HCl and ether
3. customThe layers were separated
4. washthe organic layer was washed with N/10 HCl
5. extractionextracted with ether
6. additionThe ether extracts were treated with charcoal
7. dry with materialdried with magnesium sulfate
8. customEvaporation of solvents
9. customafforded a yellow oil which
10. customwas chromatographed on silica gel using 10% CH3OH, 40% CH2Cl2, 50% Et2O as eluant