Ethyl chloroformate → 1-Ethoxycarbonyl-2-(4-methoxy-2-picolylmercapto)-1H-thieno[3,4-d]imidazole

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Reaction Conditions

Reaction Steps

Under nitrogen, 1.4 g (5.0 mmol) of 2-(4-methoxy-2-picolylmercapto)-1H-thieno[3,4-d]imidazole were dissolved in 15 ml of anhydrous dimethylformamide, and 270 mg (6 mmol) of a 60% suspension of NaH in oil were added in portions, and the mixture was heated at 30°-40° C. for 10 minutes. Now, at 25° C., 0.5 ml (5 mmol) of ethyl chloroformate (95%) was added, during which the temperature increases to about 36° C. 30 minutes later the crystalline product was filtered off with suction and washed twice with diethyl ether. Melting point 154°-156° C. (decomposition).

Provenance & Evidence