858854-82-7

基本信息
3-CHLORO-2-IODOPHENOL
Phenol, 3-chloro-2-iodo-
物理化學(xué)性質(zhì)
制備方法

863870-77-3

858854-82-7
步驟3: 在25℃下,將氫氧化鈉(32.0g,800mmol)緩慢加入至含有3-氯-2-碘苯基N,N-二乙基氨基甲酸酯(57.0g,161mmol)的400mL乙醇溶液中。將反應(yīng)混合物加熱至回流狀態(tài),維持2小時(shí)。反應(yīng)完成后,通過減壓蒸餾去除乙醇溶劑。將殘余物溶解于400mL水中,隨后用石油醚進(jìn)行萃取。水相用2N鹽酸溶液中和,再用乙酸乙酯萃取。合并所有有機(jī)相,用飽和食鹽水洗滌,并以無水硫酸鈉干燥。最后,通過減壓蒸餾除去有機(jī)溶劑,得到目標(biāo)產(chǎn)物3-氯-2-碘苯酚(41.0g,定量收率)。產(chǎn)物經(jīng)1H NMR(400MHz,CDCl3)表征: δ5.58(brs,1H),6.90(dd,J = 1.2,8.4Hz,1H),7.06(dd,J = 1.2,8.0Hz,1H),7.21(t,J = 8.0 Hz,1H)。
參考文獻(xiàn):
[1] Patent: US2017/145005, 2017, A1. Location in patent: Paragraph 0368; 0375; 0376; 0377
[2] Journal of Organic Chemistry, 2005, vol. 70, # 16, p. 6548 - 6551
[3] Journal of Organic Chemistry, 2007, vol. 72, # 14, p. 5113 - 5118
[4] Organic and Biomolecular Chemistry, 2010, vol. 8, # 17, p. 3860 - 3864
[5] Journal of Organic Chemistry, 2011, vol. 76, # 9, p. 3416 - 3437