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

5synthesis methods

Product Name:2-CHLORO-4,6-DIMETHYL-5-NITRO-NICOTINONITRILE
CAS Number:6220-77-5
Molecular formula:C8H6ClN3O2
Molecular Weight:211.61

5407-93-2 Synthesis

2-hydroxy-4,6-dimethyl-5-nitronicotinonitrile

5407-93-2
12 suppliers
inquiry

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

6220-77-5
21 suppliers
inquiry

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