反应详情

To a solution of 0.90 g (3.54 mmol) of ethyl 1-methyl-2-methoxymethylthieno[2,3-d]imidazol-5-yl-carboxylate in 30 mL of ethanol were added dropwise 5 mL of 2 N sodium hydroxide solution and the mixture was stirred for 2 hours at ambient temperature. Then the solvent was distilled off in vacuo, the residue was taken up in 5 mL of water and washed with 10 mL of diethylether. The aqueous phase was acidified with 6 mL of 2N hydrochloric acid, cooled to 0° C. and the precipitated crystals are filtered off. Yield: 0.50 g (63% of theory), C9H10N2O3S (226.26); Rf value: 0.21 (silica gel; methylene chloride/ethanol=9:1+a few drops of acetic acid); mass spectrum: (M)+=226.

1. distillationThen the solvent was distilled off in vacuo
2. washwashed with 10 mL of diethylether
3. temperaturecooled to 0° C.
4. filtrationthe precipitated crystals are filtered off