化学合成。
化学合成
合成路线 1(1. 合成:349-03-1)
产率:30%
合成条件:With 2.9-dimethyl-1,10-phenanthroline; oxygen; copper (I) acetate; silver sulfate; sodium bromide In dimethyl sulfoxide at 160℃; for 24 h; Schlenk technique
实验步骤:向装有磁力搅拌器的Silak反应管中加入6.2mg硫酸银,36.3mg乙酸铜和12.5mg 2,9-二甲基-1,10-邻菲咯啉47mg 2-硝基-4-三氟甲基苯甲酸 和30.9毫克溴化钠4毫升二甲基亚砜。 在氧气存在下加热160°C反应24小时。 反应完成后,加入蒸馏水淬灭反应,用乙酸乙酯萃取3次,每次10mL,浓缩合并的有机相,得到16.2mg 2-硝基-4-三氟甲基溴苯,收率为30percent。
参考文献:
- [1] Journal of Organic Chemistry, 2016, vol. 81, # 7, p. 2794 - 2803 [2] Patent: CN107325002, 2017, A. Location in patent: Paragraph 0091 [3] Organic and Biomolecular Chemistry, 2018, vol. 16, # 30, p. 5416 - 5421
合成路线 2(2. 合成:349-03-1)
产率:38%
合成条件:With copper(I) bromide; lithium bromide In tetrahydrofuran at 160℃; for 6 h;
实验步骤:重复上述反应,但使用乙酸,乙腈或四氢呋喃代替各种浓度的苄腈(0.02,0.04,0.1和1ml / mmol)。 表14显示了结果,从中可以看出最佳浓度取决于溶剂,并且在高浓度下获得最佳结果。
参考文献:
- [1] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 12 [2] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 10-11 [3] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 10-11 [4] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 10-12 [5] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 10-11 [6] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 10-11 [7] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 10-11 [8] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 10-11 [9] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 12 [10] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 10-11 [11] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 10-11 [12] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 10-11 [13] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 10-11 [14] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 10-12 [15] Patent: US6635780, 2003, B1. Location in patent: Page/Page column 10-11