化学合成,医药中间体。
医药中间体; 有机合成中间体
合成路线 1(1. 合成:21926-00-1)
产率:100%
合成条件:Stage #1: With lithium aluminium tetrahydride In tetrahydrofuran at 0℃; for 4 h; Heating / reflux Stage #2: With water; ammonium chloride In tetrahydrofuran
实验步骤:步骤b:将氢化铝锂(6.96克,0.183摩尔)加入四氢呋喃(80毫升)和四氢-4H-噻喃-4-酮肟(8克,0.0610摩尔)(步骤a)的四氢呋喃溶液(20毫升)中 在0℃下滴加入其中。将反应混合物回流约4小时,并用饱和氯化铵溶液猝灭。 用乙酸乙酯萃取,有机层用无水硫酸钠干燥,减压浓缩,得到标题化合物。产量:8克(粗品)(100%)
参考文献:
- [1] Patent: WO2008/111009, 2008, A1. Location in patent: Page/Page column 52 [2] Patent: WO2008/111010, 2008, A1. Location in patent: Page/Page column 75 [3] Patent: US2003/232847, 2003, A1. Location in patent: Page 16 [4] Journal of Organic Chemistry, 1981, vol. 46, p. 4376 - 4383 [5] Patent: WO2013/7765, 2013, A1. Location in patent: Page/Page column 110-111 [6] Patent: WO2013/149362, 2013, A1. Location in patent: Page/Page column 59-60 [7] Patent: WO2007/46550, 2007, A1. Location in patent: Page/Page column 118 [8] Journal of the American Chemical Society, 1955, vol. 77, p. 3866,3867 [9] Patent: WO2008/33562, 2008, A2. Location in patent: Page/Page column 48-49 [10] Patent: WO2008/34860, 2008, A1. Location in patent: Page/Page column 102-103 [11] Patent: US2009/76005, 2009, A1. Location in patent: Page/Page column 21 [12] Patent: EP1486490, 2004, A1. Location in patent: Page 45 [13] Patent: EP2261213, 2010, A1. Location in patent: Page/Page column 52 [14] Patent: WO2008/145688, 2008, A2. Location in patent: Page/Page column 91 [15] Patent: WO2009/112473, 2009, A1. Location in patent: Page/Page column 63