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54113-42-7

4,5-DibroMo-Furan-2-Carboxylic Acid Ethyl Ester synthesis

2synthesis methods
-

Yield:54113-42-7 97%

Reaction Conditions:

with sulfuric acid in ethanol;Reflux;

Steps:

2A ethyl 4,5-dibromofuran-2-carboxylate

25.0 g (92.6 mmol) of 4,5-dibromofuran-2-carboxylic acid are provided in 250 ml of ethanol, 4.9 ml (92.6 mmol) of sulfuric acid (98%) are added and the mixture is heated under reflux overnight. The reaction mixture is concentrated, and a saturated aqueous sodium bicarbonate solution is added to the residue until a basic pH is established. The precipitate is collected by suction filtration, washed with water and dried under high vacuum. 26.9 g (97% of theory) of the title compound are obtained.1H-NMR (400 MHz, DMSO-d6): δ=7.62 (s, 1H), 4.30 (q, 2H), 1.29 (t, 3H).LC-MS (Method 1): Rt=2.43 min; MS (ESIpos): m/z=297 [M+H]+.

References:

US2012/22059,2012,A1 Location in patent:Page/Page column 11