反应详情

64.8 g (0.26 mol) of 3-(2-chloro-6-fluorophenyl)-2,4,6-trichloropyridine (see Example Ab), 83.6 g (0.29 mol) 2-tri-n-butylstannylpyridine and 4.8 g (5.2 mmol) tetrakistriphenylphosphinepalladium(0), dissolved in 600 ml of dimethylformamide and 400 ml 1,4-dioxane, were boiled under reflux for 8 h and then stirred at room temperature overnight. The volatile components were removed under reduced pressure, and 400 ml of water were then added, the mixture was extracted five times with in each case 150 ml of methyl tert-butyl ether and the combined extracts were washed once with 100 ml of saturated sodium chloride solution, dried over sodium sulfate and concentrated under reduced pressure. The crude product was chromatographed on silica gel using cyclohexane/ethyl acetate and triturated with n-pentane. Yield 36.0 g of a colorless solid of m.p. 45° C.

1. temperatureunder reflux for 8 h
2. customThe volatile components were removed under reduced pressure, and 400 ml of water
3. additionwere then added
4. extractionthe mixture was extracted five times with in each case 150 ml of methyl tert-butyl ether
5. washthe combined extracts were washed once with 100 ml of saturated sodium chloride solution
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe crude product was chromatographed on silica gel
9. customtriturated with n-pentane