52022-77-2

基本信息
2-(3-硝基苯基)乙-1-醇
2-(3-Nitrophenyl)
TIMTEC-BB SBB008558
3-Nitrobenzeneethanol
3-nitro-benzeneethano
2-(3-Nitrophnyl)ethanol
3-NITROPHENETHYL ALCOHOL
2-(3-Nitrophenyl)ethanol
m-nitrophenethyl alcohol
Benzeneethanol, 3-nitro-
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

1877-73-2

52022-77-2
在氮?dú)獗Wo(hù)下,將200 mg 3-硝基苯乙酸溶解于2 mL無(wú)水四氫呋喃中,緩慢滴加1 mL硼烷-四氫呋喃溶液(1 M)。反應(yīng)混合物在室溫下攪拌12小時(shí),期間通過(guò)薄層色譜(TLC)監(jiān)測(cè)反應(yīng)進(jìn)度。反應(yīng)完成后,小心滴加少量水以淬滅反應(yīng)。隨后,加入過(guò)量飽和碳酸氫鈉溶液,調(diào)節(jié)反應(yīng)體系至堿性。用乙酸乙酯進(jìn)行萃取,分離有機(jī)層,經(jīng)無(wú)水硫酸鈉干燥后過(guò)濾。濾液在減壓下濃縮,得到粗產(chǎn)物。最后,通過(guò)柱層析純化,獲得125 mg 3-硝基苯乙醇(中間體XVI),產(chǎn)率為68%。
參考文獻(xiàn):
[1] Patent: CN103787992, 2016, B. Location in patent: Paragraph 0309-0312
[2] Patent: WO2014/182829, 2014, A1. Location in patent: Page/Page column 55
[3] Patent: WO2016/191172, 2016, A1. Location in patent: Page/Page column 78
[4] Helvetica Chimica Acta, 1973, vol. 56, p. 2460 - 2479
[5] Journal of the American Chemical Society, 1982, vol. 104, # 7, p. 1937 - 1951