反应详情

A solution of 11 g of the product of Step C in 110 ml of n-butanol and 11 g of potassium hydroxide was heated for 6 hours at 120° C. and the mixture was cooled and diluted with water. The mixture was extracted with ethyl acetate and the organic phase was washed with aqueous saturated sodium chloride solution, dried and evaporated to dryness under reduced pressure. The residue was chromatographed over silica gel and was eluted with a 6-3-1 chloroform-acetone-triethylamine mixture. The distilled fraction residue was taken up in methylene chloride and the solution was filtered and evaporated to dryness under reduced pressure to obtain 8 g of 3-(3-methoxyphenyl)-1,2,5,6-tetrahydropyridine.

1. temperaturethe mixture was cooled
2. extractionThe mixture was extracted with ethyl acetate
3. washthe organic phase was washed with aqueous saturated sodium chloride solution
4. customdried
5. customevaporated to dryness under reduced pressure
6. customThe residue was chromatographed over silica gel
7. washwas eluted with a 6-3-1 chloroform-acetone-triethylamine mixture
8. filtrationthe solution was filtered
9. customevaporated to dryness under reduced pressure