化学合成。
化学合成
合成路线 1(1. 合成:42027-81-6)
产率:100%
合成条件:With potassium carbonate In ethyl bromide; acetonitrile for 16 h; Reflux
实验步骤:将2-溴乙醇(3.75g,30.00mmol),4-硝基吡唑(3.39g,30.00mmol)和K 2 CO 3(4.97g,36.00mmol)在乙腈(30mL)中的混合物回流16小时。 然后过滤混合物,将滤液浓缩至干,得到粗产物2-(4-硝基-1H-吡唑-1-基)乙醇,为白色固体(4.70g,收率:100%),其直接用于 下一步。 ESI-MS(M + H):158.0。
参考文献:
- [1] Patent: WO2015/89337, 2015, A1. Location in patent: Paragraph 0214 [2] Patent: WO2009/154769, 2009, A1. Location in patent: Page/Page column 41 [3] Patent: WO2016/42341, 2016, A1. Location in patent: Page/Page column 183; 184 [4] Patent: WO2015/48281, 2015, A1. Location in patent: Paragraph 00413; 00414 [5] Patent: US2015/336982, 2015, A1. Location in patent: Paragraph 0342; 0343 [6] Patent: WO2015/25197, 2015, A1. Location in patent: Paragraph 00080 [7] Patent: WO2007/99326, 2007, A1. Location in patent: Page/Page column 112 [8] Patent: WO2012/110986, 2012, A1. Location in patent: Page/Page column 43 [9] Patent: WO2013/17479, 2013, A1. Location in patent: Page/Page column 48 [10] Patent: US2018/208604, 2018, A1. Location in patent: Paragraph 0301-0302