Reference of 10244-24-3 , The common heterocyclic compound, 10244-24-3, name is 4,4′-(6-Chloropyrimidine-2,4-diyl)dimorpholine, molecular formula is C12H17ClN4O2, 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.
Example 4 Preparation of Buparlisib (0036) Added compound 6 (14.4 g, 0.06 mol), bis(pinacolato)diboron (compound 5) (18.2 g, 0.072 mol), DMSO (200 mL), KOAc (17.64 g, 0.18 mol) and PdCl2(PPh3)2 (4.2 g, 0.006 mol) into a second reactor, then heated the resulting mixture to 5 C. and kept the reaction for 7 hours, and then added compound 4 (17 g, 0.06 mol) into the second reactor, kept the reaction for 16 hours. Put the reaction solution into water after the reaction was finished, and large amount of solid were separated. The resulting mixture was filtered, stirred with methanol/acetone (V:V=1:1) and crystallized for 3 hours. The filter cake was dried in vacuo at 60 C. for 8 hours to obtain the buparlisib product (compound 1) as a white solid (23.15 g, yield 94%), HPLC purity: 99.2%. Mass Spectrum: M+H- 411.
The synthetic route of 10244-24-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; XU, YONG; (6 pag.)US2016/264546; (2016); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia