作为医药中间体,用于合成相关药物分子(如3-氨基甲基-5-甲基-己酸2-甲基-1-丙酰氧基-丙基酯)。
医药中间体
合成路线 1(1. 合成:58304-65-7)
产率:38%
合成条件:at 0 - 5℃; for 4 h;
实验步骤:实施例7 PGB-06(3-氨基甲基-5-甲基 - 己酸2-甲基-1-丙酰氧基 - 丙基酯)的合成步骤:将异丁醛(3g,41.6mmol)加入到丙酰氯(3.85g,41.6mmol)中 )在0-5℃的氮气氛中并搅拌4小时。 将溶液在50℃下真空蒸馏,得到2.59g无色液体丙酸1-氯-2-甲基 - 丙基酯17(产率:38%)。 1H-NMR(CDCl3,500MHz)δ1.06(t,J = 7.0Hz,6H),7.60(t,J = 7.5Hz,3H),2.13-2.17(m,1H),2.39(q,J = 7.5 Hz,2H),6.31(d,J = 4.5 Hz,1H); 13 C-NMR(CDCl 3,125MHz)δ8.66,17.25,17.36,27.49,35.19,88.61,172.16。
参考文献:
- [1] Patent: US2008/125483, 2008, A1. Location in patent: Page/Page column 9 [2] Patent: WO2009/118580, 2009, A2. Location in patent: Page/Page column 23-24 [3] Patent: US2014/56849, 2014, A1. Location in patent: Paragraph 0306-0308 [4] Patent: CN103626765, 2016, B. Location in patent: Paragraph 0402; 0404; 0405 [5] Journal of the American Chemical Society, 1921, vol. 43, p. 665 [6] Journal of Organic Chemistry USSR (English Translation), 1983, vol. 19, # 10, p. 1872 - 1875 [7] Zhurnal Organicheskoi Khimii, 1983, vol. 19, # 10, p. 2154 - 2158 [8] Patent: US2002/58644, 2002, A1 [9] Patent: US6117885, 2000, A [10] Patent: US5374615, 1994, A [11] Patent: US5380719, 1995, A [12] Patent: US4873356, 1989, A