16097-64-6

基本信息
2,4-二氯-6-三氟甲基吡啶
2,4-二氯-6-三氟甲基嘧啶
2,4-二氯-6-三氟甲基嘧啶 1G
2,4-dichloro-6-(trifluoromethyl)pyrimidine
2,4-Dichloro-6-(trifluoromethyl)-1,3-diazine
PyriMidine, 2,4-dichloro-6-(trifluoroMethyl)-
2,4-Dichloro-6-(trifluoromethyl)pyrimidine 98%
2,4-dichloro-6-(trifluoromethyl)pyrimidine ISO 9001:2015 REACH
物理化學(xué)性質(zhì)
制備方法

672-45-7

16097-64-6
2,4-二氯-6-三氟甲基嘧啶(XXVII)的合成:在干燥條件下,將6-(三氟甲基)尿嘧啶(XXVI)(10.0g,55mmol)溶于無水乙腈(50mL)中。隨后,向反應(yīng)體系中依次加入N,N-二甲基苯胺(6.5mL,51mmol)和三氯氧磷(POCl3)(19mL,204mmol)。觀察到固體幾乎完全溶解,形成深色溶液。將反應(yīng)混合物加熱至回流狀態(tài),維持回流反應(yīng)6小時(shí)。反應(yīng)完成后,停止加熱,并在減壓條件下移除揮發(fā)性組分。將殘余物溶解于乙醚(Et2O)(300mL)中,所得乙醚溶液依次用去離子水(2×200mL)洗滌,無水硫酸鎂(MgSO4)干燥,過濾后濃縮,得到2,4-二氯-6-三氟甲基嘧啶(XXVII)為黃色油狀物(11.3g,收率94%)。產(chǎn)物經(jīng)1H NMR(CDCl3)表征:δ7.7(s,1H);GC/MS分析顯示m/z(相對(duì)豐度)220(12),218(67),216(100)。
參考文獻(xiàn):
[1] Patent: US2009/93480, 2009, A1. Location in patent: Page/Page column 6-7
[2] Patent: WO2016/42452, 2016, A1. Location in patent: Page/Page column 114; 115
[3] Patent: WO2016/42453, 2016, A1. Location in patent: Page/Page column 51
[4] European Journal of Organic Chemistry, 2006, # 6, p. 1593 - 1598
[5] Patent: WO2015/191630, 2015, A1. Location in patent: Paragraph 00398