Diphenyl Ether → HCID 59861577, compound

Participants

Reaction Conditions

Reaction Steps

Compound 7 was added to 300 mL diphenyl ether (Aldrich) that had been preheated to 250° C. in a 1 L 3-neck round bottom flask. The temperature dropped to ca 240° C. for a brief time (1-2 min), after which it was brought up to 257° C. and maintained at 255-260° C. for 15 min, as the color darkened and evolution of EtOH vapor was observed. Upon cooling to room temperature, some ppt separated, but the mixture was extremely thick. The mixture was diluted 1:4 with hexane, and more ppt separated. The ppt was filtered, washed 3× hexane, and dried to afford 19.02 g product (84%) 8. Analysis (1H NMR) showed that the product was of high enough purity to be used as such in the next step.

Provenance & Evidence