Hydrochloric Acid → HCID 86662421, compound

Temperature

-78 °C

To a cooled (−78° C.) solution of 4,5-dibromonicotinic acid ethyl ester (6 g, 19 mmol) in DCM was added diisobutylaluminum hydride (1 M in toluene, 38.8 mL, 38.8 mmol) dropwise. The mixture stirred for 3 h at −78° C. 1.5 N aqueous hydrochloric acid was added at −78° C. and then the mixture stirred at room temperature for 1 h. The reaction mixture was extracted with DCM. The organic fraction was washed with brine, dried over sodium sulfate, filtered, and concentrated to afford the crude title compound, which was used without further purification.

1. stirringthe mixture stirred at room temperature for 1 h
2. extractionThe reaction mixture was extracted with DCM
3. washThe organic fraction was washed with brine
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated

ORD record

ord-1579c2e38e1344d7867afd0fce9d8d27

Source dataset

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08378104B2