Iodine → HCID 88744272, compound

Participants

Reaction Steps

The preparation was carried out in a one liter, three-necked flask fitted with a tap adaptor, a stirring rod (plus air-tight seal) and a two-necked adaptor holding a gas-balanced dropping funnel and water cooled condenser. Into this flask were placed magnesium turnings (13.2 g, 0.54 mol) and pure, dry, air-free heptane (375 cm3) in which was dissolved n-butyl chloride (3 cm3, 28 mmol). Into the dropping funnel was placed a solution of n-butyl chloride (52.3 cm3, 0.5 mol) dissolved in di-n-butyl ether (83.3 cm3, 0.5 mol). The mixture in the flask was stirred and gently heated to reflux the mixture while a little of the n-butyl chloride solution, plus a few crystals of iodine, were added. The stirring was stopped occasionally and the mixture studied to watch for fading of the deep violet iodine colouration and the formation of bubbles. After 5 to 10 minutes the start of the reaction was signalled by the disappearance of the iodine colouration. Stirring was then resumed and sufficient heat applied to keep the mixture refluxing, while the n-butyl chloride solution was added dropwise over a period of one hour. The reaction mixture was then stirred for a further four hours.

Provenance & Evidence