Equipment needed: Parr hydrogenator , mantle and round bottom flask with cooling column with a vent hose on top to divert gases producedinto alkaline water.[/i], buchner funnel, glass trays to dry, fan , heating lamp. Note: run your water with a pump in an ice chest with ice with an aquarium pump for the cooling column.
Material needed: - Ephedrine, or +Pseudoephedrine, chloroform, methanol,2% palladium in dark charcoal, acetone, Hydrogen gas, thionyl chloride acid
Place 200gr.of Ephedrine or pseudoephedrine in a 200ml or chloroform in the round bottom flask warm up a bit then add thionyl acid 50ml. Make sure you wear gloves and a mask because thionyl is nasty oh yes goggles because it likes moisture and it will make some nasty chocking gas.
The reaction will start one needs to only warm the flask and keep it low the reaction will run about an hour. Let it cool but make sure you take the vent on top of the cooling column now and then so no vacum is created and water is sucked into your mix.
Once the stuff is cooled put some acetone so that your product precipitates and later can be vacumm filtered with a buchner funnel using paper that will catch 10 microns. Once washed well and it is white allow it to dry very good .
Step two. dissolve in methanol just enough so it all dissolves and put in the liter bottle of your hydrogenator , once you put in your palladium in charcoal. Note vacummout your bottle first and wash twice with argon before you put in your dry palladium powder then flood with alcohol while you still have argon flowing into the bottle , as to keep the palladium and charcoal from lighting up, then add your methanol mix into the bottle , now you can hydrogenate, use all the precautions with the hydrogenator , it will take about 20-30 minutes to fully hydrogenate the solution then filter and reduce methanol in a rotovac or a crock pot till it gets syruppy then pour in a glass tray and allow to cool and crystalize use a fan and a light to blow off the excees HCl as it dries. Yu will get some beautiful crystals. The yield is about 60% of the starting material.
Note : I have herd that it can be done in one shot without the refluxing with thionyl, which is hard to get and a nasty stuff to work with. so itf anyone knows the solvent to use and catalyst for hydrogenation the lead will be appreciated.
You ask does it work................very well thank you! I hesitated posting this but I have read some good sharing from many people so I thought it was the right thing to do.
Note:
the reaction can be followed with thin layer cromatography, buy spotting starting material and a known finish product, the first reaction will spot high , starting low and finish in between using ammonium hydroxide and methanol 50-50 adjust so it does't spot too high , as your solvent and iodine crystals to develop the slides.
Good chemistry...........be safe!