Synthetic Route of 22536-66-9, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 22536-66-9, name is 2-Chloropyrimidine-4-carboxamide. A new synthetic method of this compound is introduced below.
A tube containing a solution of 2-chloropyrimidine-4-carboxamide (0.24 g, 1 eq) and potassium(S)-trifluoro(3- ((3-hydroxy- 1 -methyl-2-oxopyrrolidin-3y1)ethynyl)phenyl)borate (1 eq) in Ethanol (0.25 M) was purged with nitrogen before addition of Pd(OAc)2 (0.06 eq), RuPhos (0.12 eq), and Sodium Carbonate (2 eq). The tube was sealed and stuffed at 85 C for 18 hours. The reaction mixture was cooled to room temperature and extracted with dichloromethane and saturated ammonium chloride then dried with Magnesium sulfate, filtered and concentrated todryness. The crude material subjected to reverse phase purification to afford 53 mg of the title compound (10%). M+H = 337.0; 1H NMR (400 MHz, DMSO-d6) oe 9.16-9.11 (m, 1H), 8.70- 8.60 (m, 3H), 7.98 (s, 1H), 7.94 (d, J = 5.0 Hz, 1H), 7.64 – 7.54 (m, 2H), 6.47 (s, 1H), 3.40 – 3.35 (m, 2H), 2.81 (s, 3H), 2.48 – 2.43 (m, 1H), 2.25 – 2.17 (m, 1H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound,22536-66-9, 2-Chloropyrimidine-4-carboxamide, and friends who are interested can also refer to it.
Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GENENTECH, INC.; BLAQUIERE, Nicole; BURCH, Jason; CASTANEDO, Georgette; FENG, Jianwen A.; HU, Baihua; LIN, Xingyu; STABEN, Steven; WU, Guosheng; YUEN, Po-wai; WO2015/25026; (2015); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia