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1390657-37-0

3-Pyridinecarboxylic acid, 2-(bromomethyl)-4,6-dichloro-, ethyl ester synthesis

3synthesis methods
686279-09-4 Synthesis
4,6-DICHLORO-2-METHYL-NICOTINIC ACID ETHYL ESTER

686279-09-4
107 suppliers
$50.00/250mg

3-Pyridinecarboxylic acid, 2-(bromomethyl)-4,6-dichloro-, ethyl ester

1390657-37-0
4 suppliers
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Yield:-

Reaction Conditions:

with N-Bromosuccinimide;dibenzoyl peroxide in tetrachloromethane at 85; for 24 h;

Steps:

68.68C

EXAMPLE 68C ethyl 2-(bromomethyl)-4,6-dichloronicotinate To a solution of EXAMPLE 68B (30.0 g, 128 mmol) in tetrachloromethane (500 mL) was added N-bromosuccinimide (68.4 g, 384 mmol) and benzoyl peroxide (9.29 g, 38.4 mmol) and the mixture was heated at 85°C for 1 day. The mixture was cooled to ambient temperature and filtered and the filtrate was concentrated. The residue was dissolved in ethyl acetate (400 mL), washed with brine (400 mL), dried over anhydrous sodium sulfate, filtered, concentrated and purified by flash chromatography on silica gel (200-300 mesh) eluting with 80/1 petroleum ether/ethyl acetate to give the title compound. MS : 314 (M + hT).

References:

WO2012/97682,2012,A1 Location in patent:Page/Page column 126