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ChemicalBook CAS DataBase List 4-BroMo-2,6-difluorobenzaMide, 96%

4-BroMo-2,6-difluorobenzaMide, 96% synthesis

4synthesis methods
183065-68-1 Synthesis
4-Bromo-2,6-difluorobenzoic acid

183065-68-1
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$8.00/5g

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Yield:840481-49-4 93%

Reaction Conditions:

Stage #1: 4-bromo-2,6-difluorobenzoic acidwith benzotriazol-1-ol;1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride at 20; for 2 h;
Stage #2: with ammonia in water at 0; for 20 h;

Steps:

2

Step 2 4-Bromo-2, 6-dιfluoro-benzamιde[00348] To a solution of 4-bromo-2,6-difluoro-benzoic acid (2 77g, 11 7mmol) and 1 - hydroxybenzot?azole (1 74g, 12 8mmol) is added l-ethyl-3-(3'-dimethylaminopropyl)carbodiimide (2 46g, 12 9mmol) and the solution is stirred at room temperature for 2 hours After cooling at O0C is added aq NH3 (1 74mL) and the reaction mixture is stirred for an additional 20 hours The solvent is evaporated in vacuo and the residue partitioned between diethyl ether and water The aqueous phase is extracted several times with Et2θ, the organic layers are then combined, washed with IM HCl, sat NaHCO3, d?ed over MgSO4, filtered and concentrated in vacuo to afford the benzamide as a white solid (2 56g, 93%)

References:

WO2007/131991,2007,A1 Location in patent:Page/Page column 88