With the rapid development of chemical substances, we look forward to future research findings about 171887-03-9.
As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 171887-03-9, name is N-(2-Amino-4,6-dichloropyrimidine-5-yl)formamide, molecular formula is C5H4Cl2N4O, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. name: N-(2-Amino-4,6-dichloropyrimidine-5-yl)formamide
To a slurry of N-(2-amino-4,6-dichloro-5-pyrimidinyl) formamide (42g) in 2- propanol (500 ml), triethylamine (31.4g) was added at 230C. The slurry was heated to 75-8O0C. A solution of 4-amino-2-hydroxymethylbutan-l-ol (27gm, -95% purity) in a mixture of 2-propanol (120ml) and water (17.4 ml) was slowly added to the refluxing reaction mass in about 60 minutes. The mixture was stirred at 75-8O0C for 2 hrs for completion of the reaction and concentrated under reduced pressure. The resulting residue was diluted with methanol (900 ml) and treated with activated charcoal (2 g). The solution was filtered through celite and the residue was washed with methanol (80 ml). To the filtrate 10% Palladium on Carbon (50% water paste, 6g) was added. The slurry was transferred to a hydrogenation vessel and hydrogenated at ~50C and 5-6 kg/cm2 for 20 hrs. After completion of the reaction, catalyst was removed by filtration and the residue washed with methanol (50 ml). The combined filtrate was concentrated to ~130 ml under reduced pressure at < 5O0C. The concentrate was cooled to -230C and hydrogen chloride solution in methanol (54gm, 17% w/w) was added. The light yellow coloured solution was stirred for 5-10 minutes at -230C and trimethylorthoformate (96.8Og) was added. The solution was heated to about 450C and continued stirring at 45-5O0C for 4 hrs. Thereafter, a mixture of 4gm concentrated hydrochloric acid and 6 g water was added. Stirring was continued at 45-5O0C for 90 minutes, product start crystallizing after 20 minutes of stirring. The suspension was cooled to 5-80C, stirred for 60 minutes. Product was filtered and washed with prechilled methanol (30ml, O0C), and dried at 5O0C under reduced pressure to constant weight yield 27.4 g: off white powder, HPLC purity > 98.1%.
With the rapid development of chemical substances, we look forward to future research findings about 171887-03-9.
Reference:
Patent; AUROBINDO PHARMA LIMITED; WO2008/72074; (2008); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia