化学合成。
化学合成
合成路线 1(1. 合成:528882-16-8)
产率:99%
合成条件:With hydrogen In tetrahydrofuran; methanol
实验步骤:将含有步骤b的产物(3.30G,13.1MMOL),10%钯炭(300mg)和THF-MEOH(1:1 / 50ml)的底部烧瓶抽空并用氢气冲洗三次。 将混合物在氢气氛下剧烈搅拌过夜。 通过硅藻土垫过滤除去催化剂,蒸发滤液,得到白色固体产物(2.90g,99%)。 1H NMR(CDCl3)7.10(1H,t),6.62(2H,m),6.50(1H,M),3.66(2H,br s),3.22(3H,s),1.46(9H,s)。
参考文献:
- [1] Journal of Medicinal Chemistry, 2006, vol. 49, # 7, p. 2253 - 2261 [2] Patent: WO2004/101533, 2004, A1. Location in patent: Page 26 [3] Patent: WO2004/98609, 2004, A1. Location in patent: Page/Page column 24-25 [4] Patent: WO2016/20698, 2016, A1. Location in patent: Page/Page column 59; 64; 65 [5] Patent: US2011/237620, 2011, A1. Location in patent: Page/Page column 34-35 [6] Patent: US2013/197014, 2013, A1. Location in patent: Paragraph 0715; 0718 [7] Patent: US2014/179720, 2014, A1. Location in patent: Paragraph 0439; 0445 [8] Patent: US2015/174128, 2015, A1. Location in patent: Paragraph 0690