Continuously updated synthesis method about 4-Iodopyrazole

According to the analysis of related databases, 3469-69-0, the application of this compound in the production field has become more and more popular.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 3469-69-0 as follows. 3469-69-0

Step 1: 1-(1-Ethoxyethyl)-4-iodo-1H-pyrazole 4-Iodo-1H-pyrazole (3.0 g) was suspended in benzene (150 mL) and the suspension was heated while stirring. Ethyl vinyl ether (4.4 mL) was added thereto, concentrated HCl was added dropwise thereto, and the resulting mixture was stirred at 60 C. for 3 hours. After completion of the reaction, the resulting mixture was concentrated by evaporation under a reduced pressure, and the residue was neutralized using aqueous saturated sodium hydrogen carbonate (10 mL). The resulting mixture was extracted with ethyl acetate (50 mL) and the extract was washed successively with distilled water (100 mL). The organic layer was dried over anhydrous magnesium sulfate and concentrated by evaporation under a reduced pressure. The resulting residue was purified by silica gel chromatography to obtain the title compound as a transparent yellow liquid (3.0 g, yield 73%). 1H NMR (CDCl3): delta 7.54 (s, 1H), 7.41 (s, 1H), 5.40 (q, 1H, J=6.0 Hz), 3.38-3.18 (m, 2H), 1.54 (d, 3H, J=6.0 Hz), 1.05 (t, 3H, J=7.1 Hz).

According to the analysis of related databases, 3469-69-0, the application of this compound in the production field has become more and more popular.