These common heterocyclic compound, 112253-70-0, name is 2-Amino-4-bromobenzamide, 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. Safety of 2-Amino-4-bromobenzamide
PR-9 QA-4 Oxalyl dichloride (2.5 mL, 13.11 mmol) was added drop wise to a mixture of the compound PR-9 (2.5 g, 8.74 mmol), 2-amino-4-bromobenzamide (2.5 g, 10.49 mmol) in dichloromethane (20 mL) and pyridine (20 mL) at room temperature. The mixture was stirred for 1 hour at room temperature. The solvent was removed in vacuo. The residue was purified by column chromatography (petroleum ether: acetate ether=l : 1) . The obtained intermediate amide compound (0.98 g), Na2C03 (1.08 g. 10.15 mmol), H20 (5 mL) and CH3CH2OH (5 mL) were stirred for 2 hours under reflux. Most of CH3CH2OH was removed in vacuo and the obtained residue was extracted with ethyl acetate. The organic layer was dried over Na2S04 and concentrated in vacuo. The residue was washed with t-butyl methyl ether resulting in compound QA-4 (0.89 g).
The synthetic route of 2-Amino-4-bromobenzamide has been constantly updated, and we look forward to future research findings.
Reference:
Patent; JANSSEN R&D IRELAND; VANDYCK, Koen; VERSCHUEREN, Wim, Gaston; RABOISSON, Pierre, Jean-Marie, Bernard; WO2013/98313; (2013); A1;,
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