Reagents:
- 91- 99% Isopropyl Alcohol (drug store)
- MEK Methyl Ethyl Ketone (paint / hardware store)
- VM&P Naphtha - no substitutions (paint / hardware store)
- (Do Not use Colemans, pet ether, lighter fluid, etc.)
- Xylene (paint / hardware store)
Drying Aids:
- Oven dried Epsom Salts or Washing Soda (drug / food store)
- Salt (food store)
Abstract of Procedure
- Make extraction fluid.
- Place whole pills into beaker.
- Add extraction fluid.
- Heat to boiling, stirring until pills dissolve.
- Filter while hot into elemeyer flask.
- Repeat two times.
- Return combined extractions to clean beaker.
- Add Xylene
- Heat to 105 °C to boil off alcohol.
- Filter out pseudo HCl.
- Wash pseudo HCl with MEK and let dry.
Procedure
1) For every box of pills used: combine the following solvents and drying materials in a clean beaker and in the following order:
70 mL Isopropyl Alcohol
70 mL VM&P Naphtha
2 g of salt
4 g of dried epsom salts or dried washing soda
2) Stir with a glass rod for a few minutes, then let settle for 10 minutes. Depending on how much water was in the isopropyl alcohol to start with, the mixture will settle into 2 layers or 1 layer with damp solids at the bottom.
Why not use pre dried solvents to begin with? - that is perfectly ok if you have them, but I have noticed that adding the isopropyl and naphtha together almost always releases some water, no matter how dry they were ahead of time, so I would not skip this step.
3) Filter this into the elemeyer flask leaving any solids or bottom liquid layer behind and then transfer this solution into the second clean beaker.
4) Place whole pills in the third clean beaker.
Why whole pills? Don’t I need to grind them up first? - no, we are trying to keep loss to a minimum and grinding is not necessary as the isopropyl / naphtha mixture will dissolve them very well.
5) Pour 1/3 solvent mixture over pills.
6) Place the beaker on the hotplate and bring to a boil using medium hi heat. Use the small fan to keep vapors from accumulating. Stir occasionally with a glass rod until pills have dissolved into powder. Let boil for 1-2 minutes.
7) Place a funnel with filter paper in the elemeyer flask. Filter the solvent mixture while hot, leaving as much of the solids in the beaker as possible.
8) Return any solids to the beaker and repeat steps 5 through 7 two times, combining the extractions in the elemeyer flask.
9) For every box of pills used, add to the combined extractions:
- 50 mL Xylene
10) Transfer the extraction mixture back to the empty solvent beaker and place the beaker on the hotplate. Bring to a boil using the small fan to keep vapors from accumulating. Boil until the solution reaches 105 °C.
11) Using a clean funnel and filter, paper filter off the pseudo HCl while the solution is hot.
12) Rinse the pseudo HCl with a generous amount of MEK while in the funnel.
13) Remove filter and filter cake from funnel and allow to dry completely. (no more MEK smell)
14) Weight and enjoy,
yield should be between 80 % to 90 % Introduction