403-01-0 3-氟-4-羟基苯甲酸甲酯

运输信息：常温运输。危险描述：非危险化学品，海关编码2916399090

化学合成

化学合成

路线1：

• 步骤: 向含有3-氟-4-羟基苯甲酸（5.03g，32.22mmol，可商购自Sigma-Aldrich）的圆底烧瓶中加入MeOH（50.0mL）和冷硫酸（2.0mL），加热至80℃反应20.5小时，TLC监测；反应后减压蒸除溶剂，残余物用乙醚稀释，有机相依次用饱和NaHCO₃水溶液洗涤两次、盐水洗涤一次，无水硫酸钠干燥，过滤后真空蒸除有机溶剂得产物。
• 条件: 80℃；冷硫酸；TLC监测
• 收率: 87%
• 参考文献: [1] Patent: WO2010/45258, 2010, A2. Location in patent: Page/Page column 155；[2] Patent: WO2009/111056, 2009, A1. Location in patent: Page/Page column 227-228；[3] Patent: WO2008/87529, 2008, A1. Location in patent: Page/Page column 42; 43; 119-120；[4] Patent: WO2010/9290, 2010, A1. Location in patent: Page/Page column 58；[5] Patent: US2007/191603, 2007, A1. Location in patent: Page/Page column 35；[6] Molecular Crystals and Liquid Crystals, 2011, vol. 542, p. 123 - 131；[7] Patent: EP1748048, 2007, A1. Location in patent: Page/Page column 37；[8] Patent: US2008/132458, 2008, A1. Location in patent: Page/Page column 26；[9] Patent: EP2017263, 2009, A1. Location in patent: Page/Page column 227；[10] Patent: US2006/89392, 2006, A1. Location in patent: Page/Page column 39；[11] Patent: WO2016/12916, 2016, A1. Location in patent: Page/Page column 40；[12] Patent: CN107383024, 2017, A. Location in patent: Paragraph 0140

路线2：

• 步骤: 10.0g（64.1mM）3-氟-4-羟基苯甲酸与150ml 1,2-二氯乙烷、80ml甲醇和10ml浓硫酸混合，搅拌下回流5.5小时，室温搅拌12小时；反应后加入盐溶液，分离有机层，水层用二氯甲烷萃取合并有机层，用5%碳酸氢钠水溶液洗涤，盐水洗涤，无水硫酸钠干燥，过滤后滤液浓缩，加入己烷过滤得产物。