Alloferin, Roche ,UK ,1966
31 g of diallylnortoxiferine diiodide are suspended in 1 liter of water and
shaken with 1,100 ml of Amberlite IRA-400 [chloride ion form, described
Merck Index, 7th edition, Merck and Co., Inc., Rahway, New Jersey (1960),
page 1584], for 2 hours. The diiodide thereby goes into solution. The ion
exchanger is filtered off and then washed in 3 portions with a total of 1 liter of
water. The combined filtrates are then allowed to run through a column of 300
ml of Amberlite IRA-400 (chloride ion form), rinsed with 300 ml of water and
the eluate evaporated to dryness in a vacuum while excluding air. The residue
gives on recrystallization from methanol/ethanol crystalline pure colorless
diallylnortoxiferine dichloride in a yield of 18.6 g. The compound contains 5
mols of water of crystallization after equilibration in air.
