These common heterocyclic compound, 61436-88-2, name is 2-Bromo-N-methylbenzamide, 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. Formula: C8H8BrNO
Taking R = CH3 as an example, under the protection of nitrogen, the product 2-bromo-N-methylbenzamide (0.214 g, 1 mmol) obtained in step 1,Pd (PPh3) 4 (60mg, 0.05mmol), CsF (0.456g, 3mmol) dissolved in a mixture of 15mL of 1,4 dioxane and 8mL of water, Slowly add 10 mL of a 1,4-dioxane solution containing 2-formylphenylboronic acid (0.3 g, 2 mmol),Then the reaction was terminated at 80 C. for 18-24 hours. After the reaction solution was cooled to room temperature, it was extracted twice with ethyl acetate (40 mL × 2).The organic phase was collected, washed twice with saturated brine (40 mL × 2), and then dried over anhydrous sodium sulfate.A white solid was separated by flash chromatography, and 0.2 g of white crystals were obtained after recrystallization from acetonitrile with a yield of 83%.
The synthetic route of 2-Bromo-N-methylbenzamide has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Chinese Academy Of Sciences Fujian Structure Of Matter Institute; You Lei; Zha Daijun; (18 pag.)CN110734387; (2020); A;,
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