3-(二氟甲基)-1-甲基-1H-吡唑-4-羧酸合成路线 (共 18 条)
反应条件
1: With sodium hydroxide in water T=60°C; 2 h; 2: With hydrogenchloride in water T=20°C; pH=1;
参考文献
US2011/40096 A1, ;
Page/Page column 10 ;
反应条件
1: With triethylamine in 1,4-dioxane T=25 - 82°C; 3 h; 2: With sodium hydroxide in tert-butyl methyl ether; water 0.5 h; 3: With hydrogenchloride in tert-butyl methyl ether; water
参考文献
US2012/136162 A1, ;
Page/Page column 8 ;
反应条件
1: With water; sodium hydroxide T=95°C; 4 h; 2: With hydrogenchloride; water T=20°C; Cooling with ice;
参考文献
EP2128139 A1, ;
Page/Page column 31 ;
反应条件
1: N,N-dimethylamino-1,1,2,2-tetrafluoroethane With boron trifluoride diethyl etherate in 1,4-dioxane; diethyl ether T=0 - 5°C; Inert atmosphere; 2: EtOCHCHCO2Et With pyridine in 1,4-dioxane; diethyl ether T=0 - 20°C; 3: methylhydrazine
参考文献
US2010/184994 A1, ;
Page/Page column 8-9 ;
反应条件
1: N,N'-dibenzylidene-N-methylhydrazinium methylsulfate With sodium hydroxide in water; toluene T=60°C; 3 h; 2: 2-ethoxymethlene-4,4-difluoroacetoacetic acid ethyl ester With toluene-4-sulfonic acid in toluene T=20 - 60°C;
参考文献
WO2011/54733 A1, ;
Page/Page column 39 ;
反应条件
water; triethylamine; triphenylphosphine; tris(triphenylphosphonium)palladium(II)chloride in 1-methyl-pyrrolidin-2-one T=150°C; P=4500.45 - 5250.53 Torr; Product distribution / selectivity;
参考文献
EP2008996 A1, ;
Page/Page column 9; 14 ;
反应条件
1: methylhydrazine With benzaldehyde in water; toluene T=25 - 60°C; 6.16667 h; Inert atmosphere; 2: 2-ethoxymethlene-4,4-difluoroacetoacetic acid ethyl ester in water; toluene T=20 - 30°C; 19 h; Product distribution / selectivity;
参考文献
US2011/172436 A1, ;
Page/Page column 12 ;
反应条件
1: dimethyl sulfate With benzaldehyde; hydrazine hydrate in toluene T=70 - 90°C; 2: With sodium hydroxide in water; toluene T=60°C; 3 h; 3: 2-ethoxymethlene-4,4-difluoroacetoacetic acid ethyl ester Product distribution / selectivity;
参考文献
WO2011/54733 A1, ;
Page/Page column 40-41 ;
反应条件
1: N,N-dimethylamino-1,1,2,2-tetrafluoroethane With boron trifluoride diethyl etherate in 1,4-dioxane; diethyl ether T=0 - 5°C; Inert atmosphere; 2: ethyl 3-(pyrrolidin-1-yl)acrylate With pyridine in 1,4-dioxane; diethyl ether T=0 - 5°C; 3: methylhydrazine
参考文献
US2010/184994 A1, ;
Page/Page column 9 ;
反应条件
1: With sodium hydroxide in water; xylene T=15 - 25°C; 0.666667 h; 2: With sodium hydroxide; water in xylene T=65°C; 0.75 h; 3: With hydrogenchloride; water in xylene T=95°C; 0.166667 h; Product distribution / selectivity;
参考文献
EP1997808 A1, ;
Page/Page column 5 ;