Ammonia → HCID 57336666, compound

Temperature

30 °C

A 250 mL round bottom flask was charged with 5-bromo-2,4-dichloro-3-nitropyridine (3.5 g, 12.6 mmol) and a solution of ammonia in 1,4-dioxane (150 mL). The mixture was heated at 30° C. for 4 h. Work-up: the reaction mixture was concentrated in vacuo. The residue was poured into saturated aqueous NaHCO3 and extracted with EtOAc. The combined organic layers were dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was further purified by flash column chromatography on silica gel with 20% EtOAc in petroleum ether, to afford 1.5 g (46%) of the product as a white solid. MS m/z: 252 (M+H+).

1. concentrationthe reaction mixture was concentrated in vacuo
2. additionThe residue was poured into saturated aqueous NaHCO3
3. extractionextracted with EtOAc
4. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
5. concentrationconcentrated in vacuo
6. customThe residue was further purified by flash column chromatography on silica gel with 20% EtOAc in petroleum ether

ORD record

ord-a9f505e2224f475896dd2b73669f1174

Source dataset

uspto-grants-2013_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08569300B2