877264-43-2

基本信息
(5-氟-2-碘苯基)甲醇
(5-fluoro-2-iodophenyl)methano
5-Fluoro-2-iodobenzylalcohol97%
(5-Fluoro-2-iodophenyl)Methanol
Benzenemethanol, 5-fluoro-2-iodo-
5-Fluoro-2-iodobenzyl alcohol 97%
制備方法

52548-63-7

877264-43-2
步驟1:將5-氟-2-碘苯甲酸(5.00 g,18.80 mmol)溶解于四氫呋喃(50 mL)中,在氮氣保護(hù)下冷卻至0℃。在攪拌條件下,緩慢滴加硼烷-二甲基硫醚復(fù)合物(3.57 mL,37.60 mmol),隨后將反應(yīng)混合物逐漸升溫至室溫。反應(yīng)在室溫下持續(xù)攪拌16小時。反應(yīng)完成后,將混合物小心倒入冰中,并加入10%碳酸鉀水溶液(50 mL)進(jìn)行淬滅。用二氯甲烷(2×50 mL)萃取混合物,合并有機(jī)相,用硫酸鎂干燥,隨后在減壓下濃縮,得到5-氟-2-碘苯甲醇,為無色固體(4.80 g,收率91%)。1H NMR(400 MHz,CDCl3):δ7.68(dd,1H,J= Hz),7.19(dd,1H,J= Hz),6.70(td,1H,J= Hz),4.57(d,2H,J= Hz),1.95(t,1H,J= Hz)。
參考文獻(xiàn):
[1] Advanced Synthesis and Catalysis, 2015, vol. 357, # 14-15, p. 3206 - 3214
[2] Organic Letters, 2018, vol. 20, # 2, p. 345 - 348
[3] Patent: WO2013/132376, 2013, A1. Location in patent: Page/Page column 238
[4] Patent: US2006/52378, 2006, A1. Location in patent: Page/Page column 146
[5] Chemical Communications, 2013, vol. 49, # 31, p. 3254 - 3256