Chloroform → HCID 13376240, compound

Participants

Reaction Conditions

Reaction Steps

0,15 g of 5-[2-(1-imidazolyl)-1-ethoxy]-thiophene-2-carboxylic-acid methyl ester (formula I: R=H, R1 =CH3) were dissolved in 5 ml of absolute chloroform, cooled to -40° C. and 0,16 g (1,19 mol) of SO2Cl2 were dropped thereto such that the temperature did not exceed -35° C. After standing over night it was evaporated in vacuo, the residue was partioned between 2N HCl and ether, the aqueous phase was extracted several times with ether, neutralized with sodium hydrogen carbonate and extracted several times with methylene chloride. The combined methylene chloride phases were dried (sodium sulfate) and evaporated, the residue from the evaporation was separated by column chromatography (eluant: benzene/ethanol 9:1). Yield 73 mg (43%), melting point 97°-99° C. (benzene/ether), colorless crystals.

Provenance & Evidence