Phosgene → HCID 12861465, compound

Participants

Reaction Steps

A mixture of 5 g. of 4-amino-3,5-dichloroacetophenone, 5 ml. of phosgene, and 30 ml. of toluene was heated to 150° C. for 24 hours at a sealed tube. The reaction mixture obtained was cooled and concentrated under a reduced pressure to provide crude 4-acetyl-2,6-dichlorophenyl isocyanate. The crude product was dissolved in 100 ml. of toluene and after adding 10 g. of cyclohexanol to the solution, the mixture was stirred overnight at 100° C. The reaction mixture was cooled and concentrated under reduced pressure. The residue formed was then recrystallized from a mixture of benzene and n-hexane to provide 4.3 g. of 3,5-dichloro-4-cyclohexyloxycarbonylaminoacetophenone having a melting point of 88°-89° C.

Provenance & Evidence