2491-18-1 L-蛋氨酸甲酯盐酸盐
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安全说明
危险性质:非危险化学品
用途与制备
化学合成。
化学合成
67-56-1 63-68-3 2491-18-1 合成实施例1:将L-蛋氨酸(0.5 g,1当量)悬浮于装有磁力搅拌子的100 mL圆底烧瓶中,加入甲醇(30 mL,浓度为0.1 M),并在氮气氛围下冷却至0℃。缓慢滴加亚硫酰氯(0.5 mL,2当量)至上述悬浮液中,随后加热回流反应16小时。反应完成后,通过旋转蒸发仪除去溶剂,得到浅黄色固体。将该固体用热乙醚研磨,过滤去除乙醚溶液,得到白色固体L-蛋氨酸甲酯盐酸盐(0.65561 g,收率98%)。产物经真空干燥进一步纯化。1H NMR (D2O, 500 MHz) δH: 4.24 (1H, m, CH), 3.79 (3H, s, OCH3), 2.63 (2H, t, CH2), 2.25 (1H, m, CH2), 2.16 (1H, m, CH2), 2.06 (1H, s, SCH3). 13C NMR (D2O, 125 MHz) δC: 170.58 (C=O), 53.64 (OCH3), 51.70 (CH), 28.71 (CH2), 28.41 (CH2), 13.85 (SCH3). IR (neat, vmax, cm-1): 2880.8/2676.2 (CH3, CH2, CH), 2016.2, 1742.2 (C=O, ester), 1483.6, 1443.5, 1227, 1194.7, 1149.8, 1079.5 (C-O). HRMS m/z (+ESI): C6H14NO2S, calculated mass = 164.074 (error = 0.07 ppm). 参考文献: [1] Journal of Organic Chemistry, 2011, vol. 76, # 1, p. 201 - 215 [2] Journal of the American Chemical Society, 2017, vol. 139, # 40, p. 14077 - 14089 [3] Patent: WO2012/131313, 2012, A1. Location in patent: Page/Page column 49 [4] Patent: US2014/39200, 2014, A1. Location in patent: Paragraph 0376-0380 [5] Indian Journal of Chemistry - Section B Organic and Medicinal Chemistry, 2006, vol. 45, # 8, p. 1942 - 1944