2-氯-6-甲基苯甲酰氯合成路线 （共 13 条）
反应条件
1.1: dichloromethane / 15 h / 25 °C 2.1: n-hexyl lithium / hexane; tetrahydrofuran / 2.33 h / -5 - 6 °C 2.2: 3 h / -5 - 5 °C 2.3: 1 h / -5 - 14 °C 3.1: hydrogenchloride / isopropyl alcohol / 8 h / 70 °C 4.1: triethylamine / isopropyl alcohol / 24 h / 80 °C 5.1: hydrogenchloride / ethanol; water / 1.5 h / 22 - 35 °C 5.2: pH 8 - 9 View Scheme
参考文献
Ren, Pingda; Martin, Michael; Isbester, Paul; Lane, Benjamin S.; Kropp, Jason
Patent: US2012/184568 A1, 2012 ;
参考文献
Haering,M.
Helvetica Chimica Acta, 1960 , vol. 43, p. 104 - 113
反应条件
oxalyl dichloride; N,N-dimethyl-formamide in dichloromethane
T=20°C; P=760.051 Torr; 2.08333 h;
参考文献
INFINITY PHARMACEUTICALS INC.; INTELLIKINE, LLC; CASTRO, Alfredo, C.; EVANS, Catherine, A.; LESCARBEAU, Andre; LIU, Tao; SNYDER, Daniel, A.; TREMBLAY, Martin, R.; REN, Pingda; LIU, Yi; LI, Liansheng; CHAN, Katrina
Patent: WO2013/12918 A1, 2013 ;
Location in patent: Paragraph 00536; 00537 ;
WO 2013/012918 A1
反应条件
1: sodium hydrogencarbonate; bis-triphenylphosphine-palladium(II) chloride / 8 h / 140 °C / 30003 Torr / |Inert atmosphere; |Autoclave
2: sodium hydroxide; water / 21 h / |Reflux
3: oxalyl dichloride / N,N-dimethyl-formamide; toluene / 1 h / 17 °C
View Scheme
参考文献
Daniewski, Andrzej R.; Liu, Wen; Puentener, Kurt; Scalone, Michelangelo
Organic Process Research and Development, 2002 , vol. 6, # 3 p. 220 - 224
反应条件
1: sodium hydroxide; water / 21 h / |Reflux
2: oxalyl dichloride / N,N-dimethyl-formamide; toluene / 1 h / 17 °C
View Scheme
参考文献
Daniewski, Andrzej R.; Liu, Wen; Puentener, Kurt; Scalone, Michelangelo
Organic Process Research and Development, 2002 , vol. 6, # 3 p. 220 - 224
反应条件
1: base; Pd-catalyst / 160 °C / 30003 Torr / |Inert atmosphere; |Autoclave
2: sodium hydroxide; water / 21 h / |Reflux
3: oxalyl dichloride / N,N-dimethyl-formamide; toluene / 1 h / 17 °C
View Scheme
参考文献
Daniewski, Andrzej R.; Liu, Wen; Puentener, Kurt; Scalone, Michelangelo
Organic Process Research and Development, 2002 , vol. 6, # 3 p. 220 - 224
反应条件
1: base; Pd-catalyst / 30003 Torr / |Inert atmosphere; |Autoclave; |Heating
2: sodium hydroxide; water / 21 h / |Reflux
3: oxalyl dichloride / N,N-dimethyl-formamide; toluene / 1 h / 17 °C
View Scheme
参考文献
Daniewski, Andrzej R.; Liu, Wen; Puentener, Kurt; Scalone, Michelangelo
Organic Process Research and Development, 2002 , vol. 6, # 3 p. 220 - 224
反应条件
1.1: n-heptane / 1 h / 17 °C
2.1: tetrahydrofuran / 5 - 17 °C
2.2: 5 - 25 °C
3.1: sodium dihydrogen phosphate dihydrate; sodium chlorite; dihydrogen peroxide / water; acetonitrile / 10 - 19 °C
4.1: oxalyl dichloride / N,N-dimethyl-formamide; toluene / 1 h / 17 °C
View Scheme
参考文献
Daniewski, Andrzej R.; Liu, Wen; Puentener, Kurt; Scalone, Michelangelo
Organic Process Research and Development, 2002 , vol. 6, # 3 p. 220 - 224
反应条件
1: sodium dihydrogen phosphate dihydrate; sodium chlorite; dihydrogen peroxide / water; acetonitrile / 10 - 19 °C
2: oxalyl dichloride / N,N-dimethyl-formamide; toluene / 1 h / 17 °C
View Scheme
参考文献
Daniewski, Andrzej R.; Liu, Wen; Puentener, Kurt; Scalone, Michelangelo
Organic Process Research and Development, 2002 , vol. 6, # 3 p. 220 - 224
反应条件
1: aq. KOH / ethanol / Heating
2: aq. NaNO2, H2SO4
3: SOCl2
View Scheme
参考文献
Haering,M.
Helvetica Chimica Acta, 1960 , vol. 43, p. 104 - 113
