1,4-Dioxane → HCID 178420570, compound

Participants

Reaction Steps

The zinc chloride solution was charged to the flask by syringe and diluted with 60 ml THF all under a nitrogen atmosphere. The stirrer was started and phenylmagnesium bromide introduced using a dry 20 ml syringe dropwise over 5 min initially forming a precipitate which dissolved by the end of the addition. The reaction mixture was held at 20-25° C. during addition and stirred for a total of 2 hours. The dioxan was then added by syringe causing a fine, white solid to precipitate. The slurry was stirred a further 45 min at 25° C., then filtered via the in-line sintered glass filter. The filter cake was washed with 10 ml THF and blown dry with nitrogen. The filtrate was a pale yellow solution in THF of diphenylzinc (57 mol % Zn, 10.2 mol % Mg). The flask was sealed and stored in a refrigerator.

Provenance & Evidence