Electric Literature of 1245506-61-9, 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. 1245506-61-9, name is 2-Chloro-5-methoxy-4-methylpyrimidine. A new synthetic method of this compound is introduced below.
To a -78 C solution of Intermediate 3B (1.60 g, 10.09 mmol) in DCM (20 mL) was added BBr3 (3.82 mL, 40.4 mmol) dropwise. The reaction mixture was allowed to slowly warm to RT and stirred for 16 h at RT, then was cautiously quenched with satd aq. NaHC03 (pH adjusted to ~4) and partitioned between EtOAc and water. The aqueous phase was extracted with EtOAc (2x); the combined organic layers were dried (MgS04) and concentrated in vacuo. The crude product was chromato graphed (40 g S1O2; continuous gradient from 0-100% EtOAc in Hexane over 15 min) to afford the title compound (1.33 g, 9.20 mmol, 91 % yield) as a white solid. NMR (400 MHz, DMSO- d6) d 10.63 (s, 1H), 8.11 (s, 1H), 2.34 (s, 3H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound,1245506-61-9, 2-Chloro-5-methoxy-4-methylpyrimidine, and friends who are interested can also refer to it.
Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; SHI, Yan; WANG, Ying; CHENG, Peter Tai Wah; LI, Jun; WALKER, Steven J.; (147 pag.)WO2019/126089; (2019); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia