Acetone → 2,4-Diiodopyrimidin-5-amine

温度

25 °C

A 4-necked roundbottom flask was charged with acetone (9.8 L), 2,4-dichloro-5-nitropyrimidine (670 g, 3.45 mol), and sodium iodide dihydrate (1929.6 g, 10.38 mol). Hydrogen iodide (67 ml, 40%) was then added dropwise. The resulting solution was allowed to react, with stirring, for three hours while the temperature was maintained at 20-30° C. Iron (978.6 g, 17.48 mol) was then added followed by the dropwise addition of water (300 ml). The resulting solution was allowed to react, with stirring, for an additional two hours while the temperature was maintained at reflux. The resulting slurry was filtered and the filtrate was concentrated under reduced pressure. The resulting aqueous solution was extracted four times with five liters of ethyl acetate. The combined organic layers were concentrated under reduced pressure. The resulting residue was purified via silica gel chromatography eluting with 1:1 ethyl acetate/petroleum ether to afford the title compound.

1. customto react
2. customto react
3. stirringwith stirring, for an additional two hours while the temperature
4. temperaturewas maintained
5. temperatureat reflux
6. filtrationThe resulting slurry was filtered
7. concentrationthe filtrate was concentrated under reduced pressure
8. extractionThe resulting aqueous solution was extracted four times with five liters of ethyl acetate
9. concentrationThe combined organic layers were concentrated under reduced pressure
10. customThe resulting residue was purified via silica gel chromatography
11. washeluting with 1:1 ethyl acetate/petroleum ether

ORDレコード

ord-1020019b008d45e5965bb9f4053f5660

出典データセット

uspto-grants-2013_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08344144B2