丙戊酸杂质B 2,2-二-正丙基乙酸合成路线 （共 8 条）
反应条件
1: 3-methyl butyric acid With lithium diisopropyl amide in tetrahydrofuran T=-20°C; 0.25 h; 2: With N,N,N',N',N'',N''-hexamethylphosphoric triamide in tetrahydrofuran T=4°C; 0.0833333 h; 3: 1-iodo-propane in tetrahydrofuran T=0 - 20°C; 1 h; Further stages.;
参考文献
Shimshoni, Jakob Avi; Bialer, Meir; Wlodarczyk, Bogdan; Finnell, Richard H.; Yagen, Boris
Journal of Medicinal Chemistry, 2007 , vol. 50, # 25 p. 6419 - 6427
反应条件
1: C5H8O2(2-)*2Li(1+) With N,N,N',N',N'',N''-hexamethylphosphoric triamide in tetrahydrofuran; hexane T=20°C; 0.5 h; 2: 1-iodo-propane in tetrahydrofuran; hexane T=0 - 20°C; 1 h; 3: With hydrogenchloride; water in tetrahydrofuran; hexane T=0°C; pH=1 - 2;
参考文献
WO2009/1356 A2, ;
Page/Page column 33-35 ;
反应条件
1: C5H8O2(2-)*2Li(1+) With N,N'-dimethyl-N,N'-propyleneurea in tetrahydrofuran T=5°C; 0.5 h; 2: 2-iodo-propane in tetrahydrofuran T=20°C; 2 h;
参考文献
Journal of Medicinal Chemistry, , vol. 52, # 22 p. 7236 - 7248
反应条件
1: n-Pentanoic acid With lithium diisopropyl amide in tetrahydrofuran T=-15 - -5°C; Inert atmosphere; 2: With N,N'-dimethyl-N,N'-propyleneurea in tetrahydrofuran T=5°C; 0.5 h; 3: 2-iodo-propane in tetrahydrofuran T=20°C; 2 h;
参考文献
Journal of Medicinal Chemistry, , vol. 53, # 10 p. 4177 - 4186
反应条件
1: KOH / H2O; ethanol / Heating 2: 120 - 180 °C / Heating View Scheme
参考文献
Chemical Research in Toxicology, , vol. 9, # 5 p. 866 - 870
反应条件
1: sodium hydride / dimethylformamide 2: KOH / H2O; ethanol / Heating 3: 120 - 180 °C / Heating View Scheme
参考文献
Chemical Research in Toxicology, , vol. 9, # 5 p. 866 - 870
反应条件
T=120 - 180°C; Decarboxylation; Heating;
参考文献
Chemical Research in Toxicology, , vol. 9, # 5 p. 866 - 870
反应条件
potassium carbonate in water; acetone
参考文献
Shell Oil Company
Patent: US4042710 A1, 1977 ;
