3-Bromo-5-methoxypicolinonitrile synthesis
- Product Name:3-Bromo-5-methoxypicolinonitrile
- CAS Number:717843-46-4
- Molecular formula:C7H5BrN2O
- Molecular Weight:213.03
950670-18-5
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Yield:717843-46-4 1130 mg
Reaction Conditions:
in methanol at 20 - 60; for 10.5 h;Cooling with ice;Temperature;Time;
Steps:
1 [00348] Step 1 : 3-bromo-5-methoxy-pyridine-2-carbonitrile
Sodium methoxide (296 mg, 5.47 mmol) was added to an ice-cooled solution of 3-bromo-5-fluoropyridine-2-carbonitrile (1000 mg, 4.98 mmol) in Methanol (15 mL).The Reaction mixture was warmed to ambient temperature and stirred for 1.5 hours Sodium methoxide (296 mg, 5.47 mmol) was added and the RM was stirred at ambient temperature for 1 h, heated to 40°C for 4 h, then at over the weekend. Sodium methoxide (150 mg) was added and the mixture was stirred at 60°C for 4 hours. The mixture was evaporated under reduced pressure, water was added and the mixture was extracted with ethyl acetate. The combined organic extracts were washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by chromatography on SiO2 (25 g SNAP Duo; 0-100% EtOAc in heptane) to the title compound (1130 mg, 106%) as a white powder. Method A: LC-MS (electrospray): m/z = 213/ 215 (M+H)+, RT = 1.05 min
References:
WO2022/74379,2022,A1 Location in patent:Paragraph 00348-00349; 00358-00360
