157893-14-6

基本信息
3-溴-5-甲氧基苯甲酸
3-BROMO-5-METHOXYBENZOIC ACID
5-BROMO-3-METHOXYBENZOIC ACID
Benzoic acid, 3-bromo-5-methoxy-
3-Bromo-5-methoxybenzoic acid 99%
3-Bromo-5-carboxyanisole, 5-Bromo-m-anisic acid
物理化學性質(zhì)
制備方法

864293-44-7

157893-14-6
以2-氨基-5-溴-3-甲氧基苯甲酸為原料合成3-溴-5-甲氧基苯甲酸的一般步驟如下:在0℃下,將2-氨基-5-溴-3-甲氧基苯甲酸(4g,16.3mmol)溶于水(20mL)中。隨后,向該溶液中加入濃鹽酸(7.5mL,90mmol)和四氫呋喃(20mL)。將反應混合物攪拌30分鐘后,加入亞硝酸鈉(3.16g,45.8mmol)。繼續(xù)攪拌2小時后,向反應體系中加入次磷酸(5.1g,76mmol,50%水溶液)。將混合物在室溫下攪拌16小時。反應完成后,通過過濾收集沉淀物,用水洗滌,并在真空下干燥,得到目標產(chǎn)物3-溴-5-甲氧基苯甲酸(3.2g,收率85%)。產(chǎn)物經(jīng)ESI-MS分析,m/z:229.2 [M-H]?。
參考文獻:
[1] Patent: US2009/203677, 2009, A1. Location in patent: Page/Page column 53
[2] Patent: US2009/197871, 2009, A1. Location in patent: Page/Page column 53
[3] Patent: WO2009/100169, 2009, A1. Location in patent: Page/Page column 131
[4] Patent: US2014/288045, 2014, A1. Location in patent: Paragraph 0512
[5] Patent: WO2016/44772, 2016, A1. Location in patent: Paragraph 303; 304