Diphenyl Ether → HCID 178515591, compound

Participants

Reaction Conditions

Reaction Steps

Dowtherm A (a eutectic mixture of 26.5% diphenyl and 73.5% diphenyl oxide) (1.2 L) was charged into a round-bottom flask equipped with a condenser, magnetic stirrer, thermocouple, heating mantle with a variable voltage controller, and a nitrogen inlet, and heated to 250° C. To this was cautiously added in small portions 48 g (0.11 moles) of 3-(4-bromophenylamino)-3-(3-fluorophenyl)-acrylic acid butyl ester. As portions were added gas was evolved and foaming occurred. Crystals of product began to form and adhere to the sides. After all the material had been added the heating of the reaction was continued for 1 hour. The mixture was then cooled to room temperature and hexane was added. A solid product was collected by vacuum filtration and washed with hexane. After drying in a vacuum oven, 35.7 g (90%) of product was recovered.

Provenance & Evidence