Reference of 26621-44-3, A common heterocyclic compound, 26621-44-3, name is 3-Nitro-1H-pyrazole, molecular formula is C3H3N3O2, 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.
To a mixture of 3-nitro-1H-pyrazole (5 g, 44.22 mmol, 1 eq) in DMF (50 mL) was added NaH (2.12 g, 53.06 mmol, 60 wt.% in mineral oil, 1.2 eq) at 0 C. The reaction mixture was stirred at 0 C for 0.5 hour. Then 2,2-dimethyloxirane (3.51 g, 48.64 mmol, 1.1 eq) was added into the above mixture at 0 C. The resulting mixture was warmed to 25 C and stirred at 25 C for 1 hour. The reaction mixture was quenched by addition of H2O (100 mL) and extracted with EtOAc (2 x 50 mL). The combined organic layers were washed with brine (2 x 30 mL), dried over Na2SO4, filtered and concentrated under reduced pressure to give the title compound (3.7 g, crude) as yellow oil, which was used directly in the next step.1H NMR (400 MHz, CDCl3): d 7.60 (dd, 1 H), 6.93 (d, 1 H), 4.21 (s, 2 H) and 1.27 (s, 6 H). One exchangable proton not observed.LCMS: m/z 208.1 (M+Na)+(ES+)
The synthetic route of 26621-44-3 has been constantly updated, and we look forward to future research findings.