反应详情

A mixture of 2-isopropylpyridine-N-oxide (104, 1.33 g, 9.7 mmol), cyanotrimethyl-silane (TMS-CN) (1.42 mL, 1.06 g, 11.0 mmol) in 1,2-dichloroethane (40 mL) was stirred at room temperature for 5 min. Then, diethylcarbamoylchloride (Et2NCOCl, 1.23 mL, 9.7 mmol) was added and the mixture was stirred at room temperature under inert atmosphere. After 2 days, a aqueous solution of potassium carbonate (10%) was added and the stirring was continued for 10 min. The organic layer was separated, and the water layer was extracted twice with 1,2-dichloroethane. The combined organic layers were washed with brine, dried (Na2SO4) and evaporated. The residue was purified by column chromatography on silica gel (Hexanes/AcOEt, 3:1) to give 1.06 g (74%) of the title compound: m/z=147 (M+H)+.

1. stirringthe mixture was stirred at room temperature under inert atmosphere
2. waitAfter 2 days
3. waitthe stirring was continued for 10 min
4. customThe organic layer was separated
5. extractionthe water layer was extracted twice with 1,2-dichloroethane
6. washThe combined organic layers were washed with brine
7. dry with materialdried (Na2SO4)
8. customevaporated
9. customThe residue was purified by column chromatography on silica gel (Hexanes/AcOEt, 3:1)