化学合成。
医药
合成路线 1(1. 合成:204205-33-4)
产率:95.3%
合成条件:With iodine(I) bromide; 1-n-butyl-3-methylimidazolim bromide In tetrahydrofuran at 40℃; for 4 h;
实验步骤:1-环丙基-2 - (2-氟苯基)-2-乙基酮17.8g(100mmol),一溴化碘62g(300mmol)和1-丁基-3-甲基溴化咪唑8.7g(40mmol)在150ml无水中的溶液 四氢呋喃在40℃下接触反应4小时,反应后,冷却至室温,加入冰水,乙酸乙酯萃取,饱和亚硫酸氢钠洗涤,浓缩有机相,用乙醇重结晶,得到1-环丙基-2-溴 - 2 - (2-氟苯基)-2-乙基酮24.5g,收率95.3%,纯度99.73%。
参考文献:
- [1] Patent: CN105884793, 2016, A. Location in patent: Paragraph 0033; 0034; 0035 [2] Patent: WO2013/14295, 2013, A1. Location in patent: Page/Page column 19-20 [3] Patent: WO2009/122440, 2009, A1. Location in patent: Page/Page column 31 [4] Patent: CN105884599, 2016, A. Location in patent: Paragraph 0025; 0062-0064 [5] Patent: CN104418718, 2018, B. Location in patent: Paragraph 0040; 0044; 0047; 0048; 0052; 0056 [6] Patent: WO2012/52788, 2012, A1. Location in patent: Page/Page column 32 [7] Patent: WO2009/68924, 2009, A1. Location in patent: Page/Page column 11; 15-16 [8] Patent: WO2009/68924, 2009, A1. Location in patent: Page/Page column 16 [9] Patent: US2003/134872, 2003, A1 [10] Patent: US2007/243243, 2007, A1. Location in patent: Page/Page column 20-21 [11] Patent: WO2009/66326, 2009, A2. Location in patent: Page/Page column 22 [12] Patent: WO2009/68924, 2009, A1. Location in patent: Page/Page column 11; 12-13; 16-17 [13] Patent: WO2009/68924, 2009, A1. Location in patent: Page/Page column 8; 11 [14] Patent: WO2009/68924, 2009, A1. Location in patent: Page/Page column 8; 11 [15] Patent: WO2009/68924, 2009, A1. Location in patent: Page/Page column 7-8 [16] Patent: WO2009/68924, 2009, A1. Location in patent: Page/Page column 7-8 [17] Patent: WO2009/68924, 2009, A1. Location in patent: Page/Page column 7-8 [18] Patent: WO2009/68924, 2009, A1. Location in patent: Page/Page column 11; 14-15 [19] Patent: WO2009/62044, 2009, A2. Location in patent: Page/Page column 41 [20] Patent: WO2011/42918, 2011, A2. Location in patent: Page/Page column 44 [21] Patent: WO2011/92720, 2011, A2. Location in patent: Example 7 [22] Patent: WO2012/1486, 2012, A1. Location in patent: Page/Page column 17 [23] Patent: WO2012/23145, 2012, A2. Location in patent: Page/Page column 7 [24] Patent: EP2471795, 2012, A1. Location in patent: Page/Page column 4 [25] Patent: US2012/142927, 2012, A1. Location in patent: Page/Page column 2 [26] Patent: US2012/202066, 2012, A1. Location in patent: Page/Page column 21 [27] Patent: US2012/202066, 2012, A1. Location in patent: Page/Page column 23 [28] Patent: WO2014/114964, 2014, A2. Location in patent: Page/Page column 16 [29] Patent: WO2017/221187, 2017, A1. Location in patent: Page/Page column 13