3-Nitrophenyl isocyanate → 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 dissolve it therein, and the resulting solution was cooled to -5° C. 65.6 g of metanitrophenyl isocyanate dissolved in 200 ml of acetonitrile was added dropwise. During this period, the mixture was stirred while cooling so that the temperature did not exceed -5° C. In addition, 300 ml of acetonitrile was added, and the resulting mixture was stirred at 0° C. for 3 hours. Crystals formed were filtered off and wash with acetonitrile and then washed with methanol. The crystals thus obtained were dissolved in 1 liter of N,N-dimethylformamide. An insoluble portion was filtered off. To the filtrate, 3 liters of methanol was added, and the resulting solution was cooled to thereby form crystals. These crystals were filtered off and washed with acetonitrile and then washed with methanol. The yield was 98.5 g.

Provenance & Evidence