1441673-92-2
1441673-92-2 结构式
基本信息
雷迪帕维中间体2
(S)-5-(叔丁氧羰基)-5-氮杂螺[2.4]庚烷-6-羧酸钾
(S)-5-(叔丁氧基羰基)-5-氮杂螺[2.4]庚烷-6-羧酸钾
(S)-5-(叔丁氧羰基)-5-氮杂螺[2.4]庚烷-6-羧酸钾盐
(6S)-5-氮杂螺[2.4]庚烷-5,6-二甲酸 5-叔丁酯 钾盐
1)(6S)-5-氮杂螺[2.4]庚烷-5,6-二甲酸 5-叔丁酯钾盐(1:1)
(S)-5-(叔丁氧羰基)-5-氮杂螺[2.4]庚烷-6-羧酸钾 1441673-92-2
edipasvir interMediate
(6S)-5-Azaspiro[2.4]heptane-5,6-dicarboxylic acid 5-(1,1-dim...
potassiuM (S)-5-(tert-butoxycarbonyl)-5-azaspiro[2.4]heptane-6-carboxylate
(6S)-5-Azaspiro[2.4]heptane-5,6-dicarboxylic acid 5-(1,1-diMethylethyl) ester
(6S)-5-Azaspiro[2.4]heptane-5,6-dicarboxylic acid 5-(1,1-diMethylethyl) ester potassiuM salt
(6S)?-?5-?Azaspiro[2.4]?heptane-?5,?6-?dicarboxylicacid5-?(1,?1-?dimethylethyl)esterpotassiumsal
5-Azaspiro[2.4]heptane-5,6-dicarboxylic acid, 5-(1,1-dimethylethyl) ester, potassium salt, (6S)-
(6S)-5-Azaspiro[2.4]heptane-5,6-dicarboxylic acid 5-(1,1-dimethylethyl) ester potassium salt (1:1)
5-Azaspiro[2.4]heptane-5,6-dicarboxylic acid, 5-(1,1-dimethylethyl) ester, potassium salt (1:1), (6S)-
制备方法
![(S)-5-(叔丁氧羰基)-5-氮杂螺[2.4]庚烷-6-羧酸](/CAS/20150408/GIF/1129634-44-1.gif)
1129634-44-1
1441673-92-2
E. 钾盐形成 将(S)-5-(叔丁氧羰基)-5-氮杂螺[2.4]庚烷-6-羧酸（219 g）溶解于2-甲基四氢呋喃（880 mL）中，随后将溶液加热至35℃。在保持内部温度不超过40℃的条件下，缓慢加入1.0 M叔丁醇钾的THF溶液（1.05 L）。将反应混合物搅拌约30分钟，随后在约2小时内缓慢冷却至20℃。在20℃下老化1小时后，进行过滤操作。用2-甲基四氢呋喃（715 mL）洗涤滤饼。将所得固体置于真空烘箱中，于40℃下干燥24小时，得到白色固体状的(S)-5-(叔丁氧羰基)-5-氮杂螺[2.4]庚烷-6-羧酸钾（212 g，收率86%）。 1H NMR (400 MHz, CDCl3) δ 4.07 (t, J = 7.3 Hz, 1H), 3.44 (d, J = 10.4 Hz, 1H), 3.35 (s, 1H), 3.10 (d, J = 10.4 Hz, 1H), 2.03 (dd, J = 12.3, 6.9 Hz, 1H), 1.89 (dd, J = 12.3, 8.0 Hz, 1H), 1.38 (s, 9H), 0.71-0.27 (m, 4H)。 1H NMR (400 MHz, d6-DMSO) δ: 3.89 (dd, J = 8.6, 4.1 Hz, 0.4H, 旋转异构体1), 3.85 (dd, J = 8.6, 4.3 Hz, 0.6H, 旋转异构体2), 3.21-3.07 (m, 2H), 2.00-1.92 (m, 1H), 1.75-1.71 (m, 1H), 1.36 (s, 4H, 旋转异构体1), 1.32 (s, 5H, 旋转异构体2), 0.46-0.37 (m, 4H)。 13C NMR (100 MHz, d6-DMSO) δ 174.5, 174.4, 154.1, 153.4, 77.2, 76.9, 62.3, 62.0, 54.1, 53.8, 38.7, 28.4, 28.3, 20.6, 19.9, 18.8, 11.6, 10.5, 10.2。
参考文献：
[1] Patent: US2013/324496, 2013, A1. Location in patent: Paragraph 0236-0237
[2] Patent: CN104478791, 2017, B. Location in patent: Paragraph 0069; 0070; 0071; 0072