Synthetic Route of 56-06-4 ,Some common heterocyclic compound, 56-06-4, molecular formula is C4H6N4O, 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.
Synthesis of Compound (37)Intermediate AA (0.5g, 3.96 mmol) was added to a solution of NaOAc (0.647g, 4.76 mmol, 1.2 eq.) in H20 (15 mL). The reaction was heated to 60 C for ~15 minutes, and a solution of 50% aqueous ClCH2CHO (0.5 mL) was then added. The reaction stirred for 2 hours at 60 C. The reaction mixture was filtered to remove undissolved material, and the filtrate stored at 0 C overnight. The resulting precipitated solid was collected by filtration, washed with cold H20, and dried to obtain Compound (37) (120mg, 20%) as a pink solid. Rf = 0.7 (30%MeOH/CHCl3/0.2 mL of aqueous NH3). 1H-NMR (400MHz, DMSO-_¾ delta 10.95 (br. s, exchanged with D20, 1H), 10.20 (s, exchanged with D20, 1H), 6.60 (dd, J = 3.2, 2.0Hz, 1H), 6.18 (dd, J = 3.2, 2.0Hz, 1H), 6.03 (br. s, exchanged with D20, 2H). Mass (m/z): 150.8 (M++l). LCMS: (Column: Zodiacsil 120-5-C-18-Aq (4.6 * 50 mm), Mobile phase: A: 0.01M HCOONH4 (Aq); B: MeOH, T/%B: 0/5, 10/90, 10.1/5, Flow: 1.0 mL/min, Diluent: MeOH), Rt=2.599 min, 99.16 (214 nm), 99.10 (254 nm).
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. 56-06-4, 2,6-Diaminopyrimidin-4(1H)-one, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; HERCULES TECHNOLOGY MANAGEMENT CO V, INC.; BLAGG, Julian; WO2011/35009; (2011); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia