832715-51-2

基本信息
N-異丙氧羰基-4-羥基哌啶
1-異丙氧羰基-4-羥基哌啶
isopropyl 4-hydroxypiperidine-1-carboxylate
propan-2-yl 4-hydroxypiperidine-1-carboxylate
4-hydroxypiperidine-1-carboxylic acid iPr ester
4-HYDROXYPIPERIDINE-1-CARBOXYLIC ACID ISOPROPYL ESTER
4-Hydroxy-1-piperidinecarboxylic acid 1-methylethyl ester
1-Piperidinecarboxylic acid,4-hydroxy-,1-methylethyl ester
物理化學(xué)性質(zhì)
制備方法

5382-16-1

108-23-6

832715-51-2
以4-羥基哌啶和氯甲酸異丙酯為原料合成4-羥基哌啶-1-甲酸異丙酯的一般步驟: 步驟3: 4-羥基哌啶-1-甲酸異丙酯(5)的制備 在攪拌條件下,向含有4-羥基哌啶(53.8 g,1.000當(dāng)量)、三乙胺(71.8 g,1.334當(dāng)量)和乙酸乙酯(498.8 g)的混合溶液中緩慢加入純凈的氯甲酸異丙酯(78.0 g,1.1966當(dāng)量),控制加入速度以確保反應(yīng)混合物溫度維持在10°C至17°C之間(通過反應(yīng)器夾套冷卻實(shí)現(xiàn))。加料完畢后,將反應(yīng)混合物在20°C下持續(xù)攪拌18小時(shí)。隨后,加入水(100 g)并攪拌15分鐘,之后進(jìn)行相分離。在分離含水層之前,用兩份100 g的20 wt% NaCl水溶液以150 rpm的攪拌速度洗滌有機(jī)相各15分鐘。最后,用水(100 g)洗滌有機(jī)相后,將有機(jī)相在減壓條件下通過旋轉(zhuǎn)蒸發(fā)器濃縮,得到淺琥珀色油狀產(chǎn)物(2)(91.1 g,產(chǎn)率92.0%),其GC純度為96.8%。粗產(chǎn)物在117°C至120°C、0.3至1.0托的壓力下進(jìn)行蒸餾,得到無色油狀產(chǎn)物(2),回收率為95.7%,收集溫度為112°C至119°C。
參考文獻(xiàn):
[1] Patent: US2006/154940, 2006, A1. Location in patent: Page/Page column 17-18
[2] Patent: US2006/155129, 2006, A1. Location in patent: Page/Page column 14-15
[3] Patent: WO2008/8895, 2008, A1. Location in patent: Page/Page column 66; 67
[4] Patent: EP2399914, 2011, A1. Location in patent: Page/Page column 91
[5] Patent: WO2008/5576, 2008, A1. Location in patent: Page/Page column 27-28