2-BROMO-5-FLUORO-3-NITROPYRIDINE

A total of 117 g of 5-80 was divided in 4 batches of 30 g.x.3 and 27 g.x.1 and treated with POBr3 (3 equiv.; 163 g.x.3 and 155 g.x.1) and a catalytic amount of DMF (15 ml) at rt (DMF was added carefully gas evolution). After 5 min. at room temperature, the solutions were heated at 110° C. for 3 hr. LC/MS showed starting material had been consumed. The reaction mixtures were allowed to cool to rt. The reaction flasks were placed in an ice bath; and then ice was added very slowly and carefully portionwise into the flask, gas evolution was due to HBr formation; the liquid and black solid that formed was poured into a beaker with ice. EtOAc was added and the mixture was then extracted several times with EtOAc. The organic layer was washed with saturated aq. NaHCO3; H2O and brine; dried over Na2SO4 and filtered. The product was dried in the pump overnight to provide 123 g of 6-80 as a brown solid (77percent yield). [1498] Note: Reaction is completed within 1 h. [1499] 1HNMR(δ, CDCl3):8.52 (m, 1H), 7.93 (m, 1H).A total of 117 g of intermediate 4 was divided in 4 batches of 30 g.x.3 and 27 g.x.1 and treated with POBrA total of 117 g of 5-80 was divided in 4 batches of 30 g.x.3 and 27 g.x.1 and treated with POBr

Molecular Weight:220.98
XLogP3:1.8
Hydrogen Bond Acceptor Count:4
Exact Mass:219.92837
Monoisotopic Mass:219.92837
Topological Polar Surface Area:58.7
Heavy Atom Count:11
Complexity:163
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes