16298-03-6
51171-02-9
以3-氨基吡嗪-2-羧酸甲酯為原料合成甲基-3-溴吡嗪-2-羧酸甲酯的一般步驟:在0℃條件下,將溴(3.91 g,24.46 mmol)緩慢滴加到含有3-氨基吡嗪-2-羧酸甲酯(1.27 g,8.29 mmol)和氫溴酸(4.70 mL,41.5 mmol)的攪拌混合物中。隨后,滴加亞硝酸鈉(1.44 g,20.9 mmol)溶于水(6 mL)的溶液。反應(yīng)混合物在0℃下繼續(xù)攪拌15分鐘。反應(yīng)完成后,用飽和碳酸氫鈉水溶液調(diào)節(jié)pH至8,隨后用乙酸乙酯(80 mL)和氯仿(50 mL)進(jìn)行萃取。合并有機相,用無水硫酸鎂干燥,減壓濃縮,得到1.13 g(產(chǎn)率63%)橙色油狀物,靜置后固化為目標(biāo)產(chǎn)物甲基-3-溴吡嗪-2-羧酸甲酯。
參考文獻(xiàn):
[1] Patent: WO2006/91506, 2006, A2. Location in patent: Page/Page column 47
[2] Patent: WO2006/49681, 2006, A2. Location in patent: Page/Page column 45-46
[3] Patent: WO2006/121588, 2006, A2. Location in patent: Page/Page column 51
[4] Patent: WO2006/121860, 2006, A2. Location in patent: Page/Page column 51
[5] Patent: WO2006/121904, 2006, A1. Location in patent: Page/Page column 51