To a 100 ml RBF containing a mixture of 2,54 g (10 mmol) iodine, 3,12 g silver sulfate (10 mmol) and 20 ml EtOH was added 0,91 gram of 2,5-dimethoxyphenylethylamine (5 mmol) dissolved in 20 ml EtOH.
After stirring for 30 hours the now bright yellow mixture was stripped from solvents. The residue was dissolved in 30 ml CH2CL2 and the solids where filtered off.
The organic phase was washed once with 15 ml 5% aqeous NaOH, once with 15 ml H2O and dried over MgSO4. After removal of the solvents the residue was dissolved in 30 ml acetonitrille and neutralized with aqueous HCl which resulted in the formation of solids. The crystals where washed twice with acetonitrille to provide white crystals weighing 0,36 g (20%). Mp: 244-247 °C
The yields are pretty bad but i'm fairly sure these are all bad technique on my side and the reaction was stirred for 30 hours instead of 17 because of severe weekend partying
Does anybody know if the recovered solids which are presumably silver iodide as it is a yellow solid can be converted back to the sulphate just by the addition of sulphuric acid? Or is does it first need to bee converted back to silver nitrate ?