该产物可直接用于后续反应(具体应用场景需结合参考文献进一步验证)
医药; 农药
合成路线1
- 原料:异烟酸甲酯(23821-37-6)、乙腈(75-05-8)
- 步骤:在氮气保护下,将3g(22mmol)异烟酸甲酯溶解于30mL无水甲苯中;缓慢加入1.75g(44mmol)50-60% NaH(分散于矿物油中);在90℃条件下缓慢滴加5.39mL(103mmol)干燥乙腈;反应混合物加热回流18小时,产物以钠盐形式析出;冷却至室温,过滤收集固体产物;将固体溶于水,用6N HCl调节pH至5-6,以二氯甲烷(DCM)萃取产物;水相再次调节pH至4-5,用DCM二次萃取;合并有机相,经无水硫酸钠干燥后浓缩,得到粗产物。
- 条件:氮气保护;90℃;回流18小时
- 收率:58%
- 参考文献:[1] Patent: WO2008/87529, 2008, A1. Location in patent: Page/Page column 113;[2] Patent: WO2007/98826, 2007, A2. Location in patent: Page/Page column 47-48;[3] Bioorganic and Medicinal Chemistry Letters, 2009, vol. 19, #24, p. 6890-6892;[4] Patent: WO2006/84015, 2006, A2. Location in patent: Page/Page column 86-87;[5] Patent: WO2010/9290, 2010, A1. Location in patent: Page/Page column 143-144;[6] Patent: WO2010/104933, 2010, A1. Location in patent: Page/Page column 262;[7] Journal of Medicinal Chemistry, 2012, vol. 55, #10, p. 4806-4823;[8] Patent: WO2015/42085, 2015, A2. Location in patent: Page/Page column 30-31;[9] Patent: WO2015/39333, 2015, A1. Location in patent: Page/Page column 31; 32;[10] Patent: WO2015/143653, 2015, A1. Location in patent: Page/Page column 46; 47