Synthesis
General procedure for the synthesis of 2-methyl-3-nitro-5-bromobenzoic acid from 2-methyl-3-nitrobenzoic acid: N-bromosuccinimide (15 g, 84.3 mmol) was added to a concentrated sulfuric acid solution (60 mL) containing 2-methyl-3-nitrobenzoic acid (15 g, 82.8 mmol). The reaction mixture was stirred at room temperature overnight. Upon completion of the reaction, the reaction solution was slowly poured into ice water (400 mL). The precipitate was collected by filtration and dried under vacuum to give 21 g of the target product 2-methyl-3-nitro-5-bromobenzoic acid in 98% yield.
References
[1] Patent: US2012/264734, 2012, A1. Location in patent: Page/Page column 100
[2] Patent: WO2012/142513, 2012, A1. Location in patent: Page/Page column 288
[3] Patent: US2014/107122, 2014, A1. Location in patent: Paragraph 0157; 0158
[4] Patent: WO2003/99275, 2003, A1. Location in patent: Page 101
[5] Patent: US2007/219212, 2007, A1. Location in patent: Page/Page column 23