反应详情

A mixture of 22.7 g of 3-(4-methyl-pentenyl)pyridine and 22.8 g of 2-nitrobenzeneacetonitrile in 80 mL of acetic acid was cooled to 12°-13° C. and then 16 mL of sulfuric acid was added dropwise over 6 minutes. The reaction was stirred for 2 hours at ambient temperature, then after the acetic acid was removed in vacuo, 1 L of water was added and the mixture was extracted with dichloromethane to remove neutral impurities. The aqueous layer was basified with 10N sodium hydroxide, and extracted with dichloromethane (4×200 mL). The dried (K2CO3) extracts were evaporated to give 35.6 g of N-[1,1-dimethyl-(3-pyridyl)butyl]-2-nitrobenzeneacetamide. A portion was crystallized from ethyl acetate-hexane to yield the analytical sample, mp 117°-118.5° C.

1. temperaturewas cooled to 12°-13° C.
2. customafter the acetic acid was removed in vacuo, 1 L of water
3. additionwas added
4. extractionthe mixture was extracted with dichloromethane
5. customto remove neutral impurities
6. extractionextracted with dichloromethane (4×200 mL)
7. dry with materialThe dried (K2CO3) extracts
8. customwere evaporated