27652-89-7

基本信息
4-氯苯基-2-吡啶甲醇
(4-氯苯基)吡啶-2-甲醇
Α-(4-氯苯基)-2-吡啶甲醇
Α-(4-氯苯環(huán))-2-吡啶甲醇
Α-(4-氯苯基)吡啶-2-甲醇
(4-氯苯基)-吡啶-2-基甲醇
(4-氯苯基)-吡啶-2-基-甲醇
(4-氯苯基)(吡啶-2-基)甲醇
(4-氯苯基)-(2-吡啶基)甲醇
NSC 31264
Einecs 248-592-1
Carbinoxamine Impurity A
4-Chlorophenyl-2-pyridinylmethanol
a-(4-Chlorophenyl)-2-pyridinemethanol
α-(p-Chlorophenyl)-2-pyridinemethanol
((4-Chlorophenyl)-2-pyridinemethanol)
α-(4-chlorophenyl)pyridine-2-methanol
(4-Chlorophenyl)(pyridin-2-yl)Methanol
物理化學(xué)性質(zhì)
制備方法

1121-60-4

106-39-8

27652-89-7
在氬氣保護(hù)下,將鎂屑(5.37 g,223.75 mmol,3.0當(dāng)量)懸浮于無水四氫呋喃(60 mL)中,加入碘晶體(2顆)和1,2-二溴乙烷(2滴)引發(fā)反應(yīng)。隨后,在室溫下緩慢滴加4-溴氯苯(25.76 g,134.39 mmol,1.8當(dāng)量)的無水四氫呋喃溶液,滴加過程持續(xù)1小時。滴加完畢后,繼續(xù)在室溫下攪拌反應(yīng)混合物1小時。接著,在相同溫度下逐滴加入吡啶-2-甲醛(8 g,74.68 mmol)的無水四氫呋喃(19 mL)溶液,滴加完成后繼續(xù)攪拌2小時。反應(yīng)完成后,用飽和氯化銨水溶液淬滅反應(yīng),并用乙酸乙酯萃取。合并有機(jī)相,依次用水和飽和食鹽水洗滌,無水硫酸鈉干燥,過濾后減壓濃縮。通過硅膠柱色譜法純化,以40%乙酸乙酯/己烷為洗脫劑,得到(4-氯苯基)(吡啶-2-基)甲醇12.26 g,產(chǎn)率75%。ESI-MS: m/z 220 ([M+H]+)。
參考文獻(xiàn):
[1] Bioorganic and Medicinal Chemistry Letters, 2005, vol. 15, # 12, p. 3044 - 3047
[2] Journal of Medicinal Chemistry, 2007, vol. 50, # 2, p. 219 - 232
[3] Patent: WO2016/100823, 2016, A1. Location in patent: Page/Page column 115; 116
[4] Patent: US2006/100243, 2006, A1. Location in patent: Page/Page column 7; sheet 1