2-(4-(环丙基硫代)苯基)-2-氧代乙酸乙酯合成路线 (共 7 条)
反应条件
1: oxalic acid monoethyl ester chloride With AlCl3, aluminium chloride in dichloromethane T=0 - 2°C; 0.666667 h; 2: cyclopropyl phenyl sulphide in dichloromethane T=0 - 20°C; 2.75 h;
参考文献
Prosidion Ltd
Patent: WO2007/51845 A1, 2007 ;
Location in patent: Page/Page column 11 ;
反应条件
1: oxalic acid monoethyl ester chloride With AlCl3, aluminium chloride in dichloromethane T=0 - 2°C; 0.666667 h; 2: cyclopropyl phenyl sulphide in dichloromethane T=0 - 20°C;
参考文献
PROSIDION LIMITED
Patent: WO2006/16174 A1, 2006 ;
Location in patent: Page/Page column 12 ;
WO 2006/016174 A1
反应条件
1: chlorooxo ethylacetate With AlCl3, aluminium chloride in dichloromethane T=0°C; 0.75 h; Inert atmosphere; 2: cyclopropyl phenyl sulphide in dichloromethane T=25°C; 2 h;
参考文献
EP2402327 A1, ;
Page/Page column 29-30 ;
反应条件
1: 4-THP-CH2PPh3I With lithium hexamethyldisilazane in tetrahydrofuran
T=0 - 20°C; Wittig olefination; 3 h; Large scale reaction;
2: ethyl 2-(4-(cyclopropylthio)phenyl)-2-oxoacetate in tetrahydrofuran
T=0 - 20°C; Wittig olefination; Large scale reaction; Further stages;
参考文献
Magnus, Nicholas A.; Braden, Timothy M.; Buser, Jonas Y.; Debaillie, Amy C.; Heath, Perry C.; Ley, Christopher P.; Remacle, Jacob R.; Varie, David L.; Wilson, Thomas M.
Organic Process Research and Development, 2012 , vol. 16, # 5 p. 830 - 835
反应条件
1.1: lithium hexamethyldisilazane / tetrahydrofuran / 3 h / 0 - 20 °C / Large scale reaction
1.2: 0 - 20 °C / Large scale reaction
2.1: bis(norbornadiene)rhodium(I) tetrafluoroborate; (R)-(S)-MOD-Mandyphos; hydrogen; triethylamine / methanol / 4 h / 20 °C / 4380.18 Torr / Inert atmosphere; Autoclave
View Scheme
参考文献
Magnus, Nicholas A.; Braden, Timothy M.; Buser, Jonas Y.; Debaillie, Amy C.; Heath, Perry C.; Ley, Christopher P.; Remacle, Jacob R.; Varie, David L.; Wilson, Thomas M.
Organic Process Research and Development, 2012 , vol. 16, # 5 p. 830 - 835
反应条件
1: With sodium hydroxide; water in toluene
T=50 - 60°C; 4 h;
2: With hydrogenchloride in water; toluene
T=20°C; pH=7; 18 h;
参考文献
Bristol-Myers Squibb Company
Patent: US2008/9465 A1, 2008 ;
Location in patent: Page/Page column 63 ;
US 20080009465 A1
反应条件
3-chloro-benzenecarboperoxoic acid in dichloromethane
T=5 - 20°C; 2 h;
参考文献
Dunlap, Jeanette Tower; Stephenson, Gregory Alan
Patent: US2009/181981 A1, 2009 ;
Location in patent: Page/Page column 4; 5 ;