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2-CHLORO-4,6-DIMETHYL-5-NITRO-NICOTINONITRILE synthesis

5synthesis methods
5407-93-2 Synthesis
2-hydroxy-4,6-dimethyl-5-nitronicotinonitrile

5407-93-2
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Yield:6220-77-5 80%

Reaction Conditions:

with phosphorus pentachloride;trichlorophosphate at 100; for 20 h;

Steps:

A.vi.b Step b: Synthesis of 2-chloro-4,6-dimethyl-5-nitronicotinonitrile

Phosphorus oxychloride (64 mL, 689 mmol) was added to 4,6-dimethyl-5-nitro-2- oxo-l,2-dihydropyridine-3-carbonitrile (19.3 g, 100 mmol). To this mixture, phosphorus pentachloride (20.81 g, 100 mmol) was added and reaction mixture was heated to 100 °C for 20 h. Reaction mixture was cooled and poured in ice-water mixture. The precipitate obtained was filtered washed with water and dried to obtain 2-chloro-4,6-dimethyl-5- nitronicotinonitrile. Yield: 80 %; *H NMR (300 MHz, DMSO-d6): δ 2.61 (s, 3H), 2.56 (s, 3H); MS (ES): m/z 211.6.

References:

WO2014/207508,2014,A1 Location in patent:Page/Page column 57