O-Phenylenediamine → HCID 67005049, compound

Participants

Reaction Conditions

Reaction Steps

(2,6-Dichlorophenyl)methylcyanamide (150 mg) and phenylenediamine (81 mg) were dissolved in hexafluoro-2-propanol (1 ml) and heated at 100° C. in a closed vessel for 2 days. After a further day at 60° C. in an open vessel, the solvent was removed and the residue was purified by preparative HPLC. The product-containing fractions were combined, the acetonitrile was stripped off in a rotary evaporator, and the aqueous residue was neutralized with potassium carbonate and extracted three times with ethyl acetate. Drying over magnesium sulfate and purification with carbon were followed by evaporation to dryness. The residue was taken up in aqueous hydrochloric acid and freeze dried. 5 mg of the desired compound were obtained.

Provenance & Evidence