用于医药相关反应(具体用途需结合后续反应,此处基于合成方法及光谱纯度满足后续反应要求推断)
医药
路线1:
- 原料:6-氨基烟酸(1.0 g,7.23 mmol)、亚硫酰氯(1.6 mL,21.68 mmol)、乙醇(20 mL)
- 步骤:在60℃、惰性气氛及持续搅拌条件下,将亚硫酰氯缓慢滴加至6-氨基烟酸的乙醇悬浮液中;随后回流反应18小时
- 后处理:减压蒸馏去除挥发性组分;残余物用乙酸乙酯溶解,依次用饱和碳酸氢钠水溶液、去离子水及盐水洗涤;经无水硫酸钠干燥后浓缩
- 收率:1.15 g,收率95.8%
- 产物纯度:光谱纯度满足后续反应要求,无需进一步纯化
- 结构确认:1H NMR(DMSO-d6, 300 MHz, ppm):δ 8.49(d, J = 1.8 Hz, 1H),7.83-7.79(dd, J = 8.7, 2.7 Hz, 1H),6.83(bs, 2H),6.44(d, J = 8.7 Hz, 1H),4.26-4.18(q, J = 6.9 Hz, 2H),1.29-1.25(t, J = 6.9 Hz, 3H)
- 参考文献:[1] Bioorganic and Medicinal Chemistry, 2004, vol. 12, # 5, p. 1151 - 1175;[2] Patent: WO2007/86080, 2007, A2. Location in patent: Page/Page column 37;[3] Patent: WO2010/3048, 2010, A1. Location in patent: Page/Page column 110;[4] Patent: WO2015/105779, 2015, A1. Location in patent: Page/Page column 11; 12;[5] Patent: US2016/333005, 2016, A1. Location in patent: Paragraph 0042-0043