148430-81-3

基本信息
氧雜環(huán)丁烷-3-基甲磺酸酯
3-Oxetanol 3-Methanesulfonate
物理化學(xué)性質(zhì)
制備方法

7748-36-9

124-63-0

148430-81-3
在0℃下,向氧雜環(huán)丁烷-3-醇(5g,67.5mmol)和三乙胺(14.11mL,101mmol)的二氯甲烷(150mL)溶液中逐滴加入甲基磺酰氯(6.79mL,88mmol)。將反應(yīng)混合物在室溫下攪拌3小時。反應(yīng)完成后,過濾除去固體,濾液依次用冰水和飽和食鹽水洗滌。有機(jī)相用無水硫酸鈉干燥,隨后在減壓下濃縮,得到氧雜環(huán)丁烷-3-基甲磺酸酯(11.7g,67.5mmol,100%產(chǎn)率),為含有12.2wt%二氯甲烷的油狀物。產(chǎn)物經(jīng)1H NMR(400MHz,CDCl3)表征:δ3.06(s,3H),4.79-4.82(m,2H),4.86-4.90(m,2H),5.52-5.49(m,1H)。
參考文獻(xiàn):
[1] Patent: WO2013/55910, 2013, A1. Location in patent: Page/Page column 124; 125
[2] Patent: TW2017/8221, 2017, A. Location in patent: Page/Page column 98; 99
[3] Patent: WO2015/181186, 2015, A1. Location in patent: Page/Page column 169
[4] Journal of Medicinal Chemistry, 2017, vol. 60, # 23, p. 9769 - 9789
[5] Journal of Medicinal Chemistry, 2018, vol. 61, # 6, p. 2518 - 2532