Ethyl isocyanoacetate → HCID 21291405, compound

Participants

Reaction Conditions

Reaction Steps

6-Ethoxycarbonyl-3,4-dihydro-4-methyl-2H-1,4-benzodiazepine-2,5(1H)-dione (10 mmol) was dissolved in 25 ml dry dimethylformamide (DMF). While stirring, K-t-butoxide (12 mmol) was added and the mixture was thereafter cooled to -20° C. A -30° C. cold solution of K-t-butoxide (12 mmol) in dry DMF (15 ml) was charged with isocyano-acetic acid ethylester (12 mmol). This solution was added to the above mentioned solution, and the combined solution was stirred at room temperature for 2 hours. 2 ml of acetic was added, whereafter the solution was evaporated to dryness. The oily residue was subjected to SiO2 -purification with acetone/chloroform (1/3) as eluent. This yielded the title compound as a crystalline powder. M.p. 136.3°-139.9° C.

Provenance & Evidence