Related Products of 55314-16-4 ,Some common heterocyclic compound, 55314-16-4, molecular formula is C10H12N2O, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
3-Mercapto-4-methyl-N-(3-(4-methyl-1-1H-imidazole)-5-(trifluoromethyl)phenyl)benzamide was added to the reaction flask.(Intermediate D, 41.6 g, 0.1 mol, 1.0 eq.),3-dimethylamino-1-(3-pyridyl)-2-propen-1-one (starting material SM3, 22.9 g, 0.13 mol, 1.3 eq.),Potassium carbonate (30.4 g, 0.22 mol, 2.2 eq.), N,N-dimethylformamide (320 mL).The reaction temperature is raised to 100 to 110 C for 20 to 30 hours.The reaction was monitored by high performance liquid chromatography, and the temperature was lowered to 0 to 10 C, water (84 g) was added, and the mixture was stirred for 1 to 2 hours.After suction filtration, the obtained solid and water (60 g) were placed in a 100 mL three-neck flask, and kept at 0 to 10 C for 1 to 2 hours.After suction filtration, the obtained solid was washed with water (18 g), and dried under vacuum at 45 to 55 C for 14 to 18 hours to give a crude compound. Add the crude compound E and (450 mL) methanol to a 500 mL reaction flask and heat to 60-65 C.After the solid is dissolved, the temperature is slowly lowered to 0 to 5 C, and the cooling time is controlled for 3 to 4 hours.After that, the mixture was stirred at 0 to 5 C for 3 to 4 hours.Filtration and washing of the solid with ice-methanol (0 – 5 C, 15 g).The solid was collected and dried under reduced pressure at 45 to 55 C for 14 to 18 hours.The target compound nilotinib 46.6 g was obtained as a white solid with a molar yield of 88%.
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 55314-16-4, 1-(3-Pyridyl)-3-(dimethylamino)-2-propen-1-one, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; Shanghai Fu Xingxing Tai Pharmaceutical Technology Co., Ltd.; Liu Xuejun; Chen Xiaodong; Hao Lu; Wu Feng; (23 pag.)CN109666023; (2019); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem