74290-66-7

基本信息
2-氨基-3,5-二溴-6-甲基吡嗪
2-AMINO-3,5-DIBROMO-6-METHYLPYRAZINE
2-Pyrazinamine, 3,5-dibromo-6-methyl-
3,5-DIBROMO-6-METHYLPYRAZIN-2-YLAMINE
物理化學(xué)性質(zhì)
制備方法

5521-56-2

74290-66-7
以2-氨基-6-甲基吡嗪為原料合成2-氨基-3,5-二溴-6-甲基吡嗪的一般步驟:在干燥的反應(yīng)瓶中,將6-甲基吡嗪-2-胺(14.40g,132mmol)和吡啶(26.0g,330mmol)溶解于二氯甲烷(DCM,300mL)中。在室溫下,緩慢滴加溴(53.00g,330mmol)的DCM溶液。滴加完畢后,將反應(yīng)混合物在室溫下攪拌過夜。反應(yīng)完成后,加入水(150mL)淬滅反應(yīng),將混合物轉(zhuǎn)移至分液漏斗中進(jìn)行液-液分配。有機(jī)相用飽和鹽水(100mL)洗滌,無水硫酸鈉干燥,過濾。濾液經(jīng)真空濃縮,得到2-氨基-3,5-二溴-6-甲基吡嗪,為黃色固體(34.01g,收率96%)。質(zhì)譜(ESI,陽離子模式)m/z:267.9 [M + H]+。
參考文獻(xiàn):
[1] Patent: WO2018/108125, 2018, A1. Location in patent: Paragraph 00500
[2] Patent: WO2008/51493, 2008, A2. Location in patent: Page/Page column 101
[3] Patent: CN106336413, 2017, A. Location in patent: Paragraph 0357; 0358; 0359; 0340
[4] Tetrahedron, 2006, vol. 62, # 26, p. 6272 - 6288
[5] Patent: WO2008/83070, 2008, A1. Location in patent: Page/Page column 85