16133-25-8

基本信息
3-PYRIDINESULFONYL CHLORIDE, HCL
3-PYRIDINESULFONYL CHLORIDE HYDROCHLORIDE
PYRIDINE-3-SULFONYL CHLORIDE HYDROCHLORIDE
PYRIDINE-3-SULPHONYL CHLORIDE HYDROCHLORIDE
3-Pyridine sulphonyl chloride
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

636-73-7

16133-25-8
以3-吡啶磺酸為原料合成吡啶-3-磺酰氯的一般步驟:將3-吡啶磺酸(10.3 g,64.8 mmol)、五氯化磷(20.82 g,100 mmol)和三氯氧磷(10 mL,109 mmol)的混合物加熱回流3小時(shí)(參考文獻(xiàn):J. Org. Chem., 1972, 1987; Chem. 1989, 54(2), 389)。反應(yīng)完成后,將混合物蒸發(fā)至干,得到黃色固體。將該固體溶于冰水和甲基叔丁基醚的混合溶劑中,隨后緩慢加入碳酸氫鈉溶液直至中和。用固體氯化鈉飽和水相后,分離有機(jī)相,并用無水硫酸鈉干燥。最后,在真空條件下除去溶劑,得到吡啶-3-磺酰氯,為橙色液體(10.85 g,產(chǎn)率94%)。質(zhì)譜分析(ISP)顯示分子離子峰為178.1 [(M + H)+]和180.0 [(M + 2 + H)+]。
參考文獻(xiàn):
[1] Journal of the American Chemical Society, 1992, vol. 114, # 12, p. 4889 - 4898
[2] Patent: US2006/217387, 2006, A1. Location in patent: Page/Page column 25
[3] Journal of Medicinal Chemistry, 1999, vol. 42, # 13, p. 2409 - 2421
[4] Patent: CN106432067, 2017, A. Location in patent: Paragraph 0090
[5] Patent: WO2016/90317, 2016, A1. Location in patent: Page/Page column 73