Synthetic Route of 139102-34-4, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 139102-34-4 as follows.
[00197] Step 1: A mixture of methyl 4-bromo-2-methoxybenzoate (2.66 g, 10.85 mmol), 28% ammonium hydroxide (25 mL, 642 mmol) and ammonium chloride (2.0 g, 37.4 mmol) was stirred at RT for 20 min and then at 50 0C. Once the material converted forms to an oil (ca. 20 min), the mixture was cooled to RT and more ammonium hydroxide (25 mL, 642 mmol) and ammonium chloride (2.0 g, 37.4 mmol) were added. Upon completion of addition, the reaction mixture was stirred at RT overnight. After this time, the mixture was heated to reflux in an open flask to drive off the excess ammonia and then cooled to RT. The mixture was neutralized with cone. HCl and then extracted with ethyl acetate. The extract was dried (Na2SO4) and then concentrated to give a residue. The residue was purified by flash chromatography (40 g silica gel cartridge; EtO Ac/Hex) to give 4-bromo-2- methoxybenzamide (510 mg, 2.22 mmol, 20 % yield) as a white solid.
According to the analysis of related databases, 139102-34-4, the application of this compound in the production field has become more and more popular.
Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; CARTER, Percy H.; CORNELIUS, Lyndon A., M.; WO2008/42925; (2008); A1;,
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