Triphenylphosphine → HCID 86737156, compound

Participants

Reaction Steps

A solution of 4.13 g (11.2 mmol) of 5,8-bis(ethylenedioxy)nonyl iodide and 2.93 g (11.2 mmol) of triphenyl phosphine in 25 ml of acetonitrile was buffered with a few drops of Hunig's Base and heated under nitrogen at 65° for 24 hours. The solvent was removed in vacuo until the resulting gum began to foam. This viscous gum was taken up in 25 ml of 3-pentanone and the resulting solution was seeded with a crystal of the salt and allowed to stand until crystallization was complete. Filtration afforded 4.98 g of salt. The mother liquors were placed in the freezer overnight and another 0.64 g of salt crystallized. Yield (5.62 g, 80%).

Provenance & Evidence