Synthetic Route of 138786-86-4, A common heterocyclic compound, 138786-86-4, name is Methyl 4-nitro-1H-pyrazole-3-carboxylate, molecular formula is C5H5N3O4, 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.
(2) Metallic sodium(6.71 g) was added carefully and slowly to thoroughly dried methanol(830 mL) and the solution was ice-cooled after the fragment of metallic sodium was completely dissolved. Compound(1)(43.61 g) was added to the solution, then methyl iodide(43.64 mL) was added and the mixture was stirred at 60-70C for 4 hours. The reaction solution was concentrated under reduced pressure, chloroform was added to the residue and the mixture was washed with a saturated aqueous sodium bicarbonate solution and brine, dried and the solvent was distilled away. The residue was purified with a silica gel column chromatography(hexane/ethyl acetate=4/1 to 1/1) to give Compound(2)(17.0 g) as a yellow oily substance and Compound(3)(26.8 g) as a colorless powder. Compound(2): APCI-MS(m/e):186[M+H]+, 1HNMR(500MHZ/DMSO-d6 )delta(ppm):3.95(s,3H),4.00(s,3H),8.37(s,1H). Compound(3): APCI-MS(m/e):186[M+H]+, 1HNMR(500MHZ/DMSO-d6 )delta(ppm):3.94(s,3H),4.00(s,3H),8.95(s,1H).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.