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. 4316-97-6, name is 4,6-Dichloro-5-methylpyrimidine, molecular formula is C5H4Cl2N2, 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. Quality Control of 4,6-Dichloro-5-methylpyrimidine
A mixture of 4,6-dichloro-5-methylpyrimidine (available from Sigma-Aldrich No.595446) (5 g, 30.70 mmol) in ammonia (7 M solution in MeOH, 15 ml, 105 mmol) was left under stirring for 40 min in a sealed vial at 140 0C. Water (300 ml) and EtOAc (600 ml) were added to the resulting white suspension and the two layers were separated. The aqueous phase was extracted with EtOAc (3 x 600 ml). The collected organic phases were dried (Na2SO4), filtered and concentrated under reduced pressure to give the title compound D3 (3.10 g, 20.73 mmol, 68% yield) as a white solid. UPLC: rt = 0.41 min, peaks observed: 144 (M+l, 100%) and 146 (M+ 1, 33%). C5H6ClN3 requires 143. 1H NMR (400 MHz, DMSO- d6) delta(ppm): 8.06 (s, 1 H), 7.09 (bs, 2 H), 2.07 (s, 3 H).
With the rapid development of chemical substances, we look forward to future research findings about 4316-97-6.
Reference:
Patent; GLAXO GROUP LIMITED; WO2009/3997; (2009); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia