2,3-二氟-4-乙氧基苯硼酸是重要的化工产品,被用作焊接剂、多功能润滑剂和阻燃剂等,在化工领域需求巨大,它常作为关键的有机合成中间体,被广泛应用于医药、化工和材料领域。
医药; 化工; 材料
路线1:
- 步骤: 向250mL三瓶中加入15.8g(0.1mol)2,3-二氟苯醚,四氢呋喃100ml,氮气置换空气,冷却至-60℃,滴加2.5M正丁基锂44ml(0.11mol),搅拌0.5h;加入11.5g(0.11mol)硼酸三甲酯,升温至-10℃,倒入5%盐酸中酸性水解(pH=1),分液,水相用100ml甲苯萃取,合并有机相,100ml×2盐水洗涤,减压蒸馏净溶剂,加50ml乙醚煮沸,冷却至室温,冰箱冷冻,过滤得16.2g(3-a),收率80%。
- 条件: Stage #1: n-butyllithium, THF, -60℃, 0.5h, inert atmosphere;Stage #2: -10℃;Stage #3: HCl, THF, water, inert atmosphere。
- 参考文献: [1] Patent: CN103086843, 2016, B. Location in patent: Paragraph 0149-0151 [2] Patent: EP2399896, 2011, A1. Location in patent: Page/Page column 36
路线2:
- 步骤: 将中间体化合物(T-2)129.5g溶解于DryTHF 500ml,冷却至-70℃,氮气氛下滴加n-BuLi 500ml,-70℃搅拌2h;滴加硼酸三甲酯的DryTHF溶液,-70℃至20℃搅拌16h;加入2N-HCl 200ml,甲苯萃取,水洗涤,饱和NaCl洗涤,无水硫酸镁干燥,减压浓缩,重结晶(庚烷:甲苯=4:1)得117.2g(T-20),收率71%。
- 条件: Stage #1: n-butyllithium, THF, -70℃, 2h, inert atmosphere;Stage #2: -70-20℃, 16h;Stage #3: HCl, THF, water。
- 参考文献: [1] Patent: EP2484658, 2012, A1. Location in patent: Page/Page column 42 [2] Patent: JP5663957, 2015, B2. Location in patent: Paragraph 0137-0138; 0140 [3] Patent: US2009/278089, 2009, A1. Location in patent: Page/Page column 13
路线3: