3-(4-溴苯基)-5-甲基-4-异噁唑羧酸合成路线 (共 5 条)
反应条件
1: With water; sodium hydroxide in tetrahydrofuran
T=20°C; 3 h;
2: With hydrogenchloride in water
pH=Ca. 3; Cooling with ice;
参考文献
INTERMUNE, INC.; BUCKMAN, Brad, O.; NICHOLAS, John, B.; EMAYAN, Kumaraswamy; SEIWERT, Scott, D.
Patent: WO2013/25733 A1, 2013 ;
Location in patent: Paragraph 0485 ;
反应条件
1.1: N-chloro-succinimide / N,N-dimethyl-formamide / 2 h / 15 - 20 °C
2.1: sodium methylate / methanol / 0.67 h / 0 - 25 °C
3.1: water; sodium hydroxide / tetrahydrofuran / 3 h / 20 °C
3.2: pH Ca. 3 / |Cooling with ice
View Scheme
参考文献
INTERMUNE, INC.; BUCKMAN, Brad, O.; NICHOLAS, John, B.; EMAYAN, Kumaraswamy; SEIWERT, Scott, D.
Patent: WO2013/25733 A1, 2013 ;
反应条件
1.1: sodium methylate / methanol / 0.67 h / 0 - 25 °C
2.1: water; sodium hydroxide / tetrahydrofuran / 3 h / 20 °C
2.2: pH Ca. 3 / |Cooling with ice
View Scheme
参考文献
INTERMUNE, INC.; BUCKMAN, Brad, O.; NICHOLAS, John, B.; EMAYAN, Kumaraswamy; SEIWERT, Scott, D.
Patent: WO2013/25733 A1, 2013 ;
反应条件
1.1: sodium hydroxide; hydroxylamine hydrochloride / ethanol / 2 h / 30 °C
2.1: N-chloro-succinimide / N,N-dimethyl-formamide / 2 h / 15 - 20 °C
3.1: sodium methylate / methanol / 0.67 h / 0 - 25 °C
4.1: water; sodium hydroxide / tetrahydrofuran / 3 h / 20 °C
4.2: pH Ca. 3 / |Cooling with ice
View Scheme
参考文献
INTERMUNE, INC.; BUCKMAN, Brad, O.; NICHOLAS, John, B.; EMAYAN, Kumaraswamy; SEIWERT, Scott, D.
Patent: WO2013/25733 A1, 2013 ;
反应条件
(i) Na, MeOH, (ii) /BRN= 973404/, (iii) aq. KOH, EtOH; Multistep reaction;
参考文献
Doyle,F.P. et al.
Journal of the Chemical Society, 1963 , p. 5838 - 5845