反应详情

3-Amino-4-(methylamino) pyridine (1.23 g), 6,6-dimethoxyhexanol (1.62 g), copper (II) acetate monohydrate (4 g), ethanol (30 ml) and water (30 ml) were mixed and then heated at 150° in a sealed tube for 3 hours. To the cold reaction mixture was added concentrated aqueous ammonia (5 cm3) and the mixture was then filtered through "Hyflo" (Trade Mark), diluted with water (50 ml) and extracted with methylene chloride (3×200 ml). The combined organic extracts were dried over Na2SO4, filtered, and evaporated under vacuum. The residue was chromatographed on silica eluting with a mixture of methylene chloride and methanol. The fractions containing the product were evaporated to leave the title compound, (0.66 g).

1. temperatureheated at 150° in a sealed tube for 3 hours
2. customTo the cold reaction mixture
3. filtrationthe mixture was then filtered through "Hyflo" (Trade Mark)
4. additiondiluted with water (50 ml)
5. extractionextracted with methylene chloride (3×200 ml)
6. dry with materialThe combined organic extracts were dried over Na2SO4
7. filtrationfiltered
8. customevaporated under vacuum
9. customThe residue was chromatographed on silica eluting with a mixture of methylene chloride and methanol
10. additionThe fractions containing the product
11. customwere evaporated