4-(2,6-二氯苯甲酰基氨基)-1H-吡唑-3-羧酸 N-[1-(甲基磺酰基)哌啶-4-基]酰胺合成路线 (共 5 条)
反应条件
1: 4-(2,6-dichlorobenzoylamino)-1H-pyrazole-3-carboxylic acid piperidin-4-yl-amide methanesulphonic salt With methanesulfonic acid in water
T=95 - 105°C; 1.33333 - 1.66667 h;
2: methanesulfonyl chloride With sodium hydrogencarbonate in water; ethyl acetate
T=15 - 25°C; 2.5 - 3.75 h;
参考文献
ASTEX THERAPEUTICS LIMITED
Patent: WO2008/1101 A2, 2008 ;
Location in patent: Page/Page column 366-367 ;
反应条件
1: 4-(2,6-dichlorobenzoylamino)-1H-pyrazole-3-carboxylic acid piperidin-4-yl-amide methanesulphonic salt With methanesulfonic acid in water
T=15 - 105°C; 1.33333 - 1.66667 h; Industry scale;
2: With sodium hydrogencarbonate in water
T=15 - 25°C;
3: methanesulfonyl chloride in water
T=15 - 25°C; 2.5 - 3.75 h; Product distribution / selectivity;
参考文献
ASTEX THERAPEUTICS LIMITED
Patent: WO2007/129066 A1, 2007 ;
Location in patent: Page/Page column 29; 75-76 ;
反应条件
triethylamine in 1,4-dioxane
T=45°C; 2 h;
参考文献
ASTEX THERAPEUTICS LIMITED
Patent: WO2008/1101 A2, 2008 ;
Location in patent: Page/Page column 369-370 ;
反应条件
benzotriazol-1-ol; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; triethylamine in N,N-dimethyl-formamide
T=20°C; 20 h; Product distribution / selectivity;
参考文献
ASTEX THERAPEUTICS LIMITED
Patent: WO2007/129066 A1, 2007 ;
Location in patent: Page/Page column 97-98 ;
反应条件
1: in water
T=15 - 105°C; 1.33333 - 1.66667 h;
2: With sodium hydrogencarbonate in water; ethyl acetate
T=15 - 25°C; 2.5 - 3.75 h; Product distribution / selectivity;
参考文献
ASTEX THERAPEUTICS LIMITED
Patent: WO2007/129062 A1, 2007 ;
Location in patent: Page/Page column 203-204 ;
WO 2007/129062 A1