化学合成。
医药
合成路线 1(1. 合成:446273-59-2)
产率:81.7%
合成条件:With bromine; sodium hydrogencarbonate In methanol at 0 - 20℃;
实验步骤:向CH 3 H(2000mL)中的3-氨基-6-氯哒嗪([CAS 5469-69-2],(200g,1538mmol)和NaHCO 3(258g,3076mmol)的溶液中加入Br 2([CAS 7726-] 在0℃下滴加95-6],369g,2308mmol),将混合物在室温下搅拌过夜,然后加入水(2000mL),过滤固体沉淀物并用水洗涤,将固体真空干燥,得到中间体。 1(260克,81.7%)。
参考文献:
- [1] Patent: WO2014/9305, 2014, A1. Location in patent: Page/Page column 29 [2] Patent: US2015/203498, 2015, A1. Location in patent: Paragraph 0155; 0156; 0157 [3] Patent: WO2009/100375, 2009, A1. Location in patent: Page/Page column 44-45 [4] Patent: WO2010/42699, 2010, A1. Location in patent: Page/Page column 114-115 [5] Journal of Medicinal Chemistry, 2012, vol. 55, # 23, p. 10414 - 10423 [6] Patent: US2013/109661, 2013, A1. Location in patent: Paragraph 0225-0226 [7] Patent: WO2013/64445, 2013, A1. Location in patent: Page/Page column 50-51 [8] Patent: WO2011/51342, 2011, A1. Location in patent: Page/Page column 67 [9] Tetrahedron Letters, 2013, vol. 54, # 8, p. 830 - 833 [10] Patent: WO2008/88881, 2008, A1. Location in patent: Page/Page column 32 [11] Patent: EP1364952, 2003, A1. Location in patent: Page/Page column 35-36 [12] Patent: US2014/275003, 2014, A1. Location in patent: Paragraph 0215; 0216 [13] Patent: WO2013/59594, 2013, A1. Location in patent: Page/Page column 74 [14] Patent: US2013/23526, 2013, A1. Location in patent: Paragraph 0885-0886 [15] Patent: US2007/78136, 2007, A1. Location in patent: Page/Page column 27 [16] Patent: WO2017/133665, 2017, A1. Location in patent: Page/Page column 50-51 [17] Patent: WO2017/133667, 2017, A1. Location in patent: Page/Page column 170 [18] Patent: WO2009/98144, 2009, A1. Location in patent: Page/Page column 68 [19] Patent: WO2010/88518, 2010, A2. Location in patent: Page/Page column 90-91 [20] Patent: US2010/222325, 2010, A1. Location in patent: Page/Page column 93 [21] Patent: WO2017/59080, 2017, A1. Location in patent: Page/Page column 216 [22] Patent: WO2012/48258, 2012, A2. Location in patent: Page/Page column 28-29 [23] Patent: WO2012/48259, 2012, A2. Location in patent: Page/Page column 36 [24] Patent: WO2009/154769, 2009, A1. Location in patent: Page/Page column 33 [25] Patent: US2017/369489, 2017, A1. Location in patent: Paragraph 0454; 0456 [26] Patent: WO2013/5041, 2013, A1. Location in patent: Page/Page column 71 [27] Patent: US2011/82138, 2011, A1. Location in patent: Page/Page column 59 [28] Patent: WO2011/137155, 2011, A1. Location in patent: Page/Page column 29-30 [29] Patent: US2011/269752, 2011, A1. Location in patent: Page/Page column 28 [30] Patent: WO2011/143646, 2011, A1. Location in patent: Page/Page column 59 [31] Patent: US2012/122838, 2012, A1. Location in patent: Page/Page column 80 [32] ACS Combinatorial Science, 2016, vol. 18, # 10, p. 651 - 654 [33] Patent: CN105237541, 2016, A. Location in patent: Paragraph 0027 [34] Patent: CN106632068, 2017, A. Location in patent: Paragraph 0012; 0013; 0014; 0015; 0016; 0017; 0018