412278-02-5

基本信息
叔-丁基 3-羥基-3-甲基吡咯烷-1-甲酸基酯
3-Hydroxy-3-methyl-pyrrolidine-1-carboxylic acid tert-butyl ester
1-Pyrrolidinecarboxylic acid, 3-hydroxy-3-methyl-, 1,1-dimethylethyl ester
物理化學(xué)性質(zhì)
常見問(wèn)題列表

75-16-1

101385-93-7

412278-02-5
在-10℃下,向30L反應(yīng)釜中加入4L無(wú)水四氫呋喃(THF)。啟動(dòng)攪拌后,依次向反應(yīng)釜中加入氯化鋅(118g,0.86mol)和氯化鋰(402g,9.5mol)。半小時(shí)后,緩慢滴加甲基溴化鎂(3mol/L)的乙醚溶液(6.4L,19.2mol)至反應(yīng)混合物中。繼續(xù)攪拌半小時(shí)。隨后,緩慢滴加1-叔丁氧碳基-3-吡咯烷酮(1600g,8.6mol)的THF溶液。通過(guò)高效液相色譜(HPLC)監(jiān)測(cè)反應(yīng)進(jìn)度,確認(rèn)反應(yīng)完成后,緩慢滴加飽和氯化銨(NH4Cl)溶液以淬滅反應(yīng)。用乙酸乙酯萃取反應(yīng)混合物,有機(jī)相用飽和氯化鈉(NaCl)水溶液洗滌,并用無(wú)水硫酸鈉干燥。最后,通過(guò)蒸發(fā)去除溶劑,得到目標(biāo)產(chǎn)物3-羥基-3-甲基吡咯烷-1-羧酸叔丁酯,為淺黃色固體(1450g),產(chǎn)率為83.8%。
參考文獻(xiàn):
[1] Patent: US2013/252938, 2013, A1. Location in patent: Paragraph 0514
[2] Patent: US2014/45896, 2014, A1. Location in patent: Paragraph 0134; 0135; 0199; 0200
[3] Patent: EP2703398, 2014, A1. Location in patent: Paragraph 0119; 0120
[4] Patent: EP2703398, 2014, A1. Location in patent: Paragraph 0173; 0174
[5] Journal of the American Chemical Society, 2015, vol. 137, # 35, p. 11270 - 11273