2267-40-5

基本信息
3-CHLOROSULFONYL-4-FLUORO-BENZOIC ACID
3-(Chlorosulphonyl)-4-fluorobenzoic acid
Benzoic acid,3-(chlorosulfonyl)-4-fluoro-
5-Carboxy-2-fluorobenzenesulphonyl chloride
2-fluoro-5-carboxybenzenesulphonyl chloride
3-(chlorosulfonyl)-4-fluorobenzoic acid(SALTDATA: FREE)
物理化學(xué)性質(zhì)
制備方法

456-22-4

2267-40-5
實(shí)施例2:2-氟-5-(4-甲氧基苯甲酰基)-苯磺酰胺的合成;將4-氟苯甲酸(8g,57mmol)緩慢加入至氯磺酸(58g,498mmol)中,隨后加入氯化鈉(10g,169mmol)。加料完畢后,將反應(yīng)混合物在160℃下加熱5小時(shí)。反應(yīng)完成后,冷卻反應(yīng)混合物并緩慢倒入冰水中。析出的白色固體沉淀經(jīng)過(guò)濾收集,并重新溶解于乙酸乙酯中。有機(jī)層用飽和氯化鈉溶液洗滌,無(wú)水硫酸鎂干燥,過(guò)濾后減壓濃縮除去溶劑。殘余物用己烷研磨,得到7g(51%收率)目標(biāo)產(chǎn)物,為白色固體。1H NMR(CDCl3):δ8.78(m,1H),8.52(m,1H),7.5(t,1H)。MS(m/z):308(M-1)。
參考文獻(xiàn):
[1] Patent: US2004/2492, 2004, A1. Location in patent: Page/Page column 48-49
[2] Patent: WO2009/118292, 2009, A1. Location in patent: Page/Page column 42-43
[3] Journal of Medicinal Chemistry, 1997, vol. 40, # 13, p. 2017 - 2034
[4] Bioorganic and medicinal chemistry, 2002, vol. 10, # 3, p. 639 - 656
[5] Journal of Medicinal Chemistry, 2005, vol. 48, # 5, p. 1596 - 1609