Electric Literature of 4316-97-6 ,Some common heterocyclic compound, 4316-97-6, molecular formula is C5H4Cl2N2, 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.
4,6-dichloro-5-methylpyrimidine (0.98 g, 6.0 mmol), 4-chloro-2-methylphenylboronic acid (2.24 g, 13 . 2 mmol), acetonitrile (100 ml) and 1 M sodium carbonate (Na 2 CO 3) (30 ml), and nitrogen bubbling was carried out for 1 hour.Thereafter, 2210 mg of PdCl 2 (PPh 3), 0.3 mmol) was added and the reaction was carried out under reflux. The reaction solution was a yellow clear solution. Disappearance of the raw material was confirmed by TLC after 3 hours.After a while, since an orange solid precipitated, suction filtration was carried out, after washing with methanol, the filtrate was dissolved in chloroform. Washed with water 150 ml × 3 times, brine 150 ml × 1 time, and evaporation was carried out. In order to remove the catalyst, silica gel column chromatography was carried out. A glass filter 17G-4 was used and 150 cc of silica gel was used.The injection solvent was toluene, and the developing solvent was hexane: ethyl acetate = 10: 3 (vol / vol). After the evaporation, 1.0 g of a white solid was obtained, and the yield was 49%. From 1 H-NMR and MS, it was confirmed that 3 MHPM-Cl (molecular weight 343) was formed.
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. 4316-97-6, 4,6-Dichloro-5-methylpyrimidine, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; YAMAGATA UNIVERSITY; SASABE, HISAHIRO; KIDO, JUNJI; KOMATSU, RYUTARO; NAKAO, KOHEI; (58 pag.)JP2018/35129; (2018); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia