9-溴-10-(1-萘基)蒽是有机合成和化工医药研发的中间体,在实验室研发过程和化工医药生产过程中主要用作OLED中间体。
9-溴-10-(1-萘基)蒽为杂环有机物,可用作医药中间体。
合成路线 1(1. 合成:400607-04-7)
产率:97.5%
合成条件:With N-Bromosuccinimide In N,N-dimethyl-formamide for 2 h;
实验步骤:在2L的4颈圆底烧瓶中,将中间体5-a(88g,0.29mol)溶解在二甲基甲酰胺(700mL)中。 此后,缓慢加入NBS(70.7g,0.4mol)的二甲基甲酰胺(200ml)溶液,然后搅拌2小时。 在反应完成后,将反应混合物与水混合以沉淀中间体5-b(108g,97.5%)。
参考文献:
- [1] Journal of Materials Chemistry, 2012, vol. 22, # 1, p. 123 - 129 [2] Patent: US2017/12214, 2017, A1. Location in patent: Paragraph 0166; 0167 [3] Chemical Communications, 2016, vol. 52, # 73, p. 10956 - 10959 [4] Patent: KR2016/90242, 2016, A. Location in patent: Paragraph 0266; 0267; 0268; 0269; 0270; 0271 [5] Patent: KR2017/55704, 2017, A. Location in patent: Paragraph 0111; 0118-0123 [6] Patent: KR2016/12846, 2016, A. Location in patent: Paragraph 0187; 0190; 0191 [7] Patent: KR2016/22081, 2016, A. Location in patent: Paragraph 0434; 0435; 0438; 0439 [8] Patent: US2014/77166, 2014, A1. Location in patent: Paragraph 0116-0117 [9] Patent: US2014/77165, 2014, A1. Location in patent: Paragraph 0116-0118 [10] Patent: JP5847151, 2016, B2. Location in patent: Paragraph 0081 [11] Patent: KR101548370, 2015, B1. Location in patent: Paragraph 0104; 0105; 0106; 0109; 0110 [12] Patent: US8357821, 2013, B2. Location in patent: Page/Page column 55; 56
合成路线 2(2. 合成:400607-04-7)
产率:80%
合成条件:With tetrakis(triphenylphosphine) palladium (0) ; potassium carbonate In tetrahydrofuran; water at 80℃; for 2 h;
实验步骤:9,10-二溴蒽(5.04g,15mmol),萘-1-硼酸(1.72g,10mmol),Pd(PPh 3)4(0.58g,0.5mmol),碳酸钾(4.15g,30mmol)和THF :将H 2 O = 2:1的溶液溶解在200ml中。在80℃下回流搅拌2小时。 然后加入40ml H 2 O,有机层用硫酸镁萃取三次,得到40ml乙醚,用硅胶柱色谱法蒸发溶剂,得到中间体B-3(3.06g,收率80%)。 它是获得的。
参考文献:
- [1] Patent: KR2016/30001, 2016, A. Location in patent: Paragraph 0341-0344 [2] Patent: CN105384613, 2016, A. Location in patent: Paragraph 0044; 0045 [3] Patent: KR2015/22269, 2015, A. Location in patent: Paragraph 0322; 0323; 0327; 0328 [4] Patent: KR2017/49295, 2017, A. Location in patent: Paragraph 0158-0163 [5] Patent: US2016/308159, 2016, A1. Location in patent: Paragraph 0021; 0022 [6] Journal of Materials Chemistry, 2010, vol. 20, # 16, p. 3186 - 3194 [7] Patent: US2016/308157, 2016, A1. Location in patent: Paragraph 0113