2,4-dichloro-6-Methylnicotinonitrile

2, 4-dihydroxy-6-methylnicotinonitrile (40 g, 266.4 mmol) was dissolved in POCl[00157] Step 3: 2, 4-dichloro-6-methylnicotinonitrile: 2, 4-dihydroxy-6- methylnicotinonitrile (40 g, 266.4 mmol) was dissolved in POCl2, 4-Dichloro-6-methylnicotinonitrile. 2, 4-dihydroxy-6-methylnicotinonitrile (40 g, 266.4 mmol) was dissolved in POCl3 (120 mL) and DMF was added(4 drops). The mixture was heated to reflux for 3 h and was then concentrated under vacuum. The residue was dissolved in EtOAc (2 L) and carefully neutralized by treatment with sat. aq. bicarbonate solution. The mixture was then filtered through Celite, the organicl ayer separated, dried over sodium sulfate and concentrated in vacuoto provide 2, 4-dichloro-6-methylnicotinonitrile (45 g, 90percent) as an off-white solid.To a solution of 2, 4-dihydroxy-6-methylnicotinonitrile (intermediate 128A, 30 g, 599.49 mmol) inPOC13 (90 ml) was added DMF (730 mg, 29.97 mmol), then the mixture was heated at 95°C for 3h. The mixture was concentrated in vacuo; the residue was dissolved in ethyl acetate (3 1) and neutralized by saturated aqueous sodium bicarbonate solution. Then the mixture was filtered and the organic layer was separated and dried over Na2SO4, filtered and concentrated in vacuo to give 2, 4-dichloro-6-methylnicotinonitrile (intermediate 129A, combined yield from 3 batches: 90 g, 80percent yield) as brown solid.‘H NMR (400 MHz, methanol-d4) ö [ppm] = 7.60 (s, 1 H), 2.58 (s, 3 H).

Molecular Weight:187.02
XLogP3:2.6
Hydrogen Bond Acceptor Count:2
Exact Mass:185.9751535
Monoisotopic Mass:185.9751535
Topological Polar Surface Area:36.7
Heavy Atom Count:11
Complexity:186
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes