Hydrochloric Acid → 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%).

1. temperaturethe suspension was heated
2. stirringthe resulting mixture was stirred at 60° C. for 3 hours
3. customAfter completion of the reaction
4. concentrationthe resulting mixture was concentrated by evaporation under a reduced pressure
5. extractionThe resulting mixture was extracted with ethyl acetate (50 mL)
6. washthe extract was washed successively with distilled water (100 mL)
7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
8. concentrationconcentrated by evaporation under a reduced pressure
9. customThe resulting residue was purified by silica gel chromatography

ORD-Eintrag

ord-94e6445547334ae2a15fb757df2d980c

Quelldatensatz

uspto-grants-2011_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08063229B2