Hydrogen chloride-ethyl acetate → HCID 54398599, compound

Ethyl 4,5-dichloro-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-imidazole-2-carboxylate obtained in Example (7b) (0.61 g, 1.79 mmol) was dissolved in ethanol (3 mL). A 4 N hydrochloric acid/ethyl acetate solution (15 mL) was added, and the mixture was heated under reflux for one hour. The reaction solution was concentrated under reduced pressure, diluted with ethyl acetate, washed with brine and dried over anhydrous sodium sulfate. Following concentration under reduced pressure, the residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=10/1, 1/1) to obtain 0.24 g of the title compound as a pale yellow oily substance (65%).

1. temperaturethe mixture was heated
2. temperatureunder reflux for one hour
3. concentrationThe reaction solution was concentrated under reduced pressure
4. additiondiluted with ethyl acetate
5. washwashed with brine
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentration under reduced pressure
8. customthe residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=10/1, 1/1)

ORD record

ord-7700ccffa0b44b7fbca6d23b7d10b584

Source dataset

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08536197B2