Dimethylformamide → HCID 20073707, compound

Participants

Reaction Conditions

Reaction Steps

200 ml of acetonitrile and 200 ml of N,N-dimethylformamide were added to 60.4 g of 2-(4-aminophenyl)-1-formylhydrazine to be dissolved, followed by cooling to -5° C. 65.6 g of metanitrophenyl isocyanate dissolved in 200 ml of acetonitrile was added dropwise thereto. During this dropwise addition, the solution was cooled with stirring so that the temperature thereof would not exceed -5° C. A further 300 ml of acetonitrile was added at 0° C., and after stirring for 3 hours, formed crystals were filtered and washed with acetonitrile and then with methanol. The thus-obtained crystals were dissolved in 1 liter of N,N-dimethylformamide, the undissolved portion was filtered off, and 3 liters of methanol was added to the filtrate, followed by cooling to form crystals. The thus-formed crystals were then filtered and washed with acetonitrile and then methanol. The yield was 98.5 g.

Provenance & Evidence