203662-51-5
203662-51-5 結(jié)構(gòu)式
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
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
toxic compounds or compounds which causing chronic effects
制備方法
79099-07-3
106-95-6
203662-51-5
a. 在氮?dú)獗Ｗo(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?？刂品磻?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(shí)。通過(guò)薄層色譜（TLC，展開(kāi)劑比例為石油醚/乙酸乙酯=2/1，體積比）監(jiān)測(cè)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(wú)水硫酸鈉干燥，過(guò)濾后減壓濃縮，得到粗產(chǎn)物。粗產(chǎn)物通過(guò)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(wú)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