Synthetic Route of 39806-90-1, A common heterocyclic compound, 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, molecular formula is C4H5IN2, 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.
Step 1 1-Methyl-4-(methylthio)-1H-pyrazole To a solution of 4-iodo-1-methyl-1H-pyrazole (0.5 mL, 5.2 mmol) in THF (2 mL) at -78 C. under an atmosphere of N2 was added isopropylmagnesium chloride (5.2 mL, 10.4 mmol) and the resulting mixture was stirred for 30 minutes. To the reaction mixture was added dimethyl disulfide (1 mL, 11 mmol). The reaction was poured into aq. sat. NH4Cl (25 mL), the layers were separated and the aqueous layer was extracted with Et2O (100 mL). The combined organic layers were dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by reverse phase preparative HPLC (Mobile Phase: A=10 mM NH4HCO3 in H2O, B=MeCN; Gradient: B=95%; 13 min; 30 mL/min; column: Xtimate Prep C18 OBD 21.2*250 mm, 10 mum) to afford the title compound (740 mg, 29%) as an off-white solid. (ES+) C5H8N2S requires: 128, found: 129 [M+H]+.
The synthetic route of 39806-90-1 has been constantly updated, and we look forward to future research findings.