反应详情

Iodine (1.64 g, 6.5 mmol) was added at room temperature to a solution of 4-propyl-6-trimethylstannanyl-pyrimidine-2-carbonitrile (2.0 g, 6.5 mmol) in THF (100 mL). The mixture was stirred at room temperature for 2 hours, then diluted with a saturated solution of sodium thiosulfate and the THF was removed under reduced pressure. The aqueous layer was extracted with ethyl acetate (3×100 ml). The combined organic layers were washed with brine, dried over sodium sulphate, filtered and concentrated under reduced pressure. The residue was chromatographed over silica gel (eluent:Cyclohexane/Ethyl acetate 5/5) to afford 4-iodo-6-propyl-pyrimidine-2-carbonitrile (1.28 g, 72%) as a colorless oil.

1. customthe THF was removed under reduced pressure
2. extractionThe aqueous layer was extracted with ethyl acetate (3×100 ml)
3. washThe combined organic layers were washed with brine
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue was chromatographed over silica gel (eluent:Cyclohexane/Ethyl acetate 5/5)