87661-20-9

基本信息
環(huán)丙烷羧酸叔丁酯
Cyclopropanecarboxylic acid, 1,1-dimethylethyl ester
2-ethyl-, 1,1-dimethylethyl ester, (2R)-1-Pyrrolidinecarboxylic acid,
物理化學(xué)性質(zhì)
制備方法

865-47-4

4023-34-1

87661-20-9
將219.1 g(1913 mmol,1當(dāng)量)叔丁醇鉀懸浮于2.5 L叔丁基甲基醚中,并將混合物冷卻至0-5℃。在60分鐘內(nèi)緩慢滴加200 g(1913 mmol,1當(dāng)量)環(huán)丙基甲酰氯,同時(shí)保持反應(yīng)溫度在0-5℃之間(使用冰-乙醇浴冷卻)。通過(guò)在線FTIR監(jiān)測(cè)反應(yīng)進(jìn)程,確保反應(yīng)受控進(jìn)行。反應(yīng)混合物在0-5℃下繼續(xù)攪拌30分鐘后,加入1 L 5%碳酸氫鈉水溶液進(jìn)行中和。分離水相,水相用500 mL叔丁基甲基醚萃取。合并有機(jī)相,用500 mL半飽和氯化鈉水溶液洗滌。有機(jī)相在減壓下(30℃/150 mbar)濃縮,得到271 g環(huán)丙甲酸叔丁酯(產(chǎn)率91%,含有8%殘留的叔丁基甲基醚)。
參考文獻(xiàn):
[1] Patent: US2009/23713, 2009, A1. Location in patent: Page/Page column 20
[2] Patent: US2010/22518, 2010, A1. Location in patent: Page/Page column 20
[3] Patent: US2010/16282, 2010, A1. Location in patent: Page/Page column 19
[4] Patent: US2011/92698, 2011, A1. Location in patent: Page/Page column 22
[5] Journal of Organic Chemistry, 2009, vol. 74, # 22, p. 8726 - 8732