Synthetic Route of 137520-99-1 ,Some common heterocyclic compound, 137520-99-1, molecular formula is C9H9Cl2NO2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
To a mixture of 2,6-dichloro-3-methylisonicotinic acid ethyl ester (10.0 g, 42.7 mmol), Example 7E and acetic acid (2.69 g, 44.9 mmol) in carbon tetrachloride (147 ml.) are added lambda/-bromosuccinimide (8.36 g, 47.0 mmol) and then benzoyl peroxide (1.03 g, 4.27 mmol). The mixture is stirred in oil bath at 60 0C under heat lamp for 5 h. The mixture is then cooled to room temperature. About half of the solvent is removed by rotary evaporation. The white succinimide solid is removed by filtration. The overweight filtrate (17 g for a theoretical 13.4 g, 42.7 mmol) is concentrated under reduced pressure and used as a crude immediately for the next step. MS(ESI) m/z 313.99. 1H NMR (400 MHz1CDCI3) delta ppm 7.72 (s, 1 H), 4.99 (s, 2 H), 4.48 (q, J=7.16 Hz, 2 H), 1.46 (t, J=7.07 Hz, 3 H).
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 137520-99-1, Ethyl 2,6-dichloro-3-methylisonicotinate, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; NOVARTIS AG; WO2009/150230; (2009); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem