223251-16-9

基本信息
醋酸巴多昔芬中間體3
4-(2-氮雜環(huán)庚烷-1-基乙氧基)芐醇
(4-(2-(氮雜環(huán)庚烷-1-基)乙氧基)苯基)甲醇
3-(4-(2-(azepan-1-yl)ethoxy)benzyl)
4-(2-Azepan-1-ylethoxy)benzyl alcohol
[4-[2-(1-azepanyl)ethoxy]phenyl]methanol
(4-(2-(azepan-1-yl)ethoxy)phenyl)Methanol
4-[2-(Hexahydro-1H-azepin-1-yl)ethoxy]- benzeneMethanol
BenzeneMethanol, 4-[2-(hexahydro-1H-azepin-1-yl)ethoxy]-
物理化學(xué)性質(zhì)
常見(jiàn)問(wèn)題列表

223251-09-0

223251-16-9
在0至5℃條件下,向攪拌中的4-(2-(氮雜環(huán)庚烷-1-基)乙氧基)苯甲醛(200g,0.72mol,1.0當(dāng)量)的甲醇(400mL)溶液中分批加入硼氫化鈉(15.6g,0.41mol,0.57當(dāng)量)。反應(yīng)混合物在此溫度下繼續(xù)攪拌30分鐘。通過(guò)薄層色譜(TLC)監(jiān)測(cè)反應(yīng)進(jìn)度,展開(kāi)劑比例為乙酸乙酯/己烷/三乙胺(3:7:1),確認(rèn)原料完全轉(zhuǎn)化為產(chǎn)物。反應(yīng)完成后,將混合物用水(400mL)稀釋,并用二氯甲烷(3×400mL)進(jìn)行萃取。合并有機(jī)相,用無(wú)水硫酸鎂干燥。隨后,在旋轉(zhuǎn)蒸發(fā)器上濃縮有機(jī)相,得到201g(100%收率)的(4-(2-(氮雜環(huán)庚烷-1-基)乙氧基)苯基)甲醇,產(chǎn)物為稠油狀。產(chǎn)物的結(jié)構(gòu)通過(guò)1H NMR(CDCl3/TMS)確認(rèn),特征峰如下:7.27(d,2H,J=8.5Hz),6.87(d,2H,J=8.5Hz),4.60(s,2H),4.05(t,2H,J=6.21Hz),2.93(t,2H,J=6.15Hz),2.77(m,4H),1.7-1.5(m,8H)。
參考文獻(xiàn):
[1] Patent: EP1212335, 2006, B1. Location in patent: Page/Page column 25
[2] Patent: CN107400087, 2017, A. Location in patent: Paragraph 0044
[3] European Journal of Medicinal Chemistry, 2011, vol. 46, # 9, p. 3858 - 3866