203662-51-5

基本信息
1-BOC-4-烯丙基-4-羥基哌啶
4-羥基-4-(2-丙烯基)哌啶-1-羧酸叔丁酯
4-Allyl-1-Boc-4-hydroxypiperidine
benzyl 4-allyl-4-hydroxypiperidine-1-carboxylate
tert-butyl 4-allyl-4-hydroxypiperidine-1-carboxylate
tert-butyl 4-hydroxy-4-(prop-2-en-1-yl)piperidine-1-carboxyl...
tert-butyl 4-hydroxy-4-(prop-2-en-1-yl)piperidine-1-carboxylate
4-Hydroxy-4-(2-propenyl)piperidine-1-carboxylic acid tert-butyl ester
1-Piperidinecarboxylic acid, 4-hydroxy-4-(2-propenyl)-, 1,1-diMethylethyl ester
1-Piperidinecarboxylic acid, 4-hydroxy-4-(2-propen-1-yl)-, 1,1-diMethylethyl ester
制備方法

79099-07-3

106-95-6

203662-51-5
a. 在氮氣保護(hù)下,將N-叔丁氧羰基-4-哌啶酮(50 g, 0.25 mol)和鋅粉(49.2 g, 0.75 mol)懸浮于四氫呋喃(500 mL)和氯化銨水溶液(2/3, 500 mL)的混合溶液中。控制反應(yīng)溫度在-10至10℃之間,緩慢滴加3-溴-1-丙烯(109.3 g, 0.90 mol)。滴加完畢后,緩慢升溫至15-40℃,繼續(xù)攪拌反應(yīng)2-5小時。通過薄層色譜(TLC,展開劑比例為石油醚/乙酸乙酯=2/1,體積比)監(jiān)測反應(yīng)進(jìn)度。反應(yīng)完成后,用乙酸乙酯(100 mL×3)萃取反應(yīng)混合物。合并有機(jī)相,用無水硫酸鈉干燥,過濾后減壓濃縮,得到粗產(chǎn)物。粗產(chǎn)物通過硅膠柱色譜純化(洗脫劑比例為石油醚/乙酸乙酯=30/1至10/1,體積比),得到無色油狀目標(biāo)化合物4-烯丙基1-Boc-4-羥基哌啶(60 g),收率為99.9%。
參考文獻(xiàn):
[1] Patent: CN105440046, 2016, A. Location in patent: Paragraph 0006
[2] Patent: WO2010/58318, 2010, A1. Location in patent: Page/Page column 25-26
[3] Patent: WO2014/139144, 2014, A1. Location in patent: Page/Page column 165
[4] Patent: US2014/288081, 2014, A1. Location in patent: Paragraph 0667; 0668; 0669
[5] Patent: WO2014/139325, 2014, A1. Location in patent: Page/Page column 178; 179