101691-94-5

基本信息
4-碘甲基四氢吡喃
4-IODOMETHYLTETRAHYDROPYRAN
4-(Iodomethyl)tetrahydropyrane
4-(IODOMETHYL)TETRAHYDRO-2H-PYRAN
(4-TETRAHYDROPYRANYL)METHYL IODIDE
4-(Iodomethyl)tetrahydro-2H-pyrane
2H-Pyran, tetrahydro-4-(iodomethyl)-
物理化学性质
制备方法

132291-95-3

101691-94-5
制备7:4-碘甲基四氢吡喃; 将制备6(4-甲磺酰氧甲基四氢吡喃,328g,1.69mol)和碘化钠(507g,3.4mol)在丙酮(3.3L)中的混合物加热回流4小时。通过薄层色谱(TLC,展开剂:乙醚)监测反应进程,发现仍有大量甲磺酸酯未反应,遂补加碘化钠(127g,0.65mol)并继续回流16小时。反应完成后,将反应混合物冷却至室温并过滤。滤饼用丙酮洗涤,干燥后,将所得固体溶于乙醚(800mL)和水(800mL)的混合溶剂中进行分配萃取。水相再用乙醚(200mL)萃取一次,合并所有乙醚萃取液,用10%硫代硫酸钠溶液(300mL)洗涤以去除碘的颜色,随后用水(300mL)洗涤。有机相经无水硫酸镁干燥后,减压浓缩除去溶剂,得到目标产物4-碘甲基四氢吡喃(365g,收率92%)。产物的核磁共振(NMR)谱图与预期结构相符。
参考文献:
[1] Patent: WO2006/16178, 2006, A1. Location in patent: Page/Page column 11-12
[2] Patent: WO2007/51845, 2007, A1. Location in patent: Page/Page column 12-13
[3] Patent: WO2006/16174, 2006, A1. Location in patent: Page/Page column 14
[4] Patent: US2008/21052, 2008, A1. Location in patent: Page/Page column 33
[5] Patent: US2008/9465, 2008, A1. Location in patent: Page/Page column 64