Pseudoephedrine Extraction

edited December 10 in Spurious Generalities
I do not own this pseudoephedrine extraction, is just a repost from erowid archives made by geezmeister.

full method snapshot: https://www.erowid.org/archive/rhodium/chemistry/pseudo.xtract.fullturps.html

EXTRACTION OF PSEUDOEPHEDRINE

Materials required:
OTC pseudoephedrine tablets
Hotplate
Fan
Pyrex evaporation dish
Funnels, cotton balls, coffee filters
Stirring rod
Non-polar solvent of choice
Mineral turps
Acetone
Alcohol of choice (methanol, ethanol, etc.)
Beakers or collection jars.

Abstract of Procedure:
Turps soak
Non-polar solvent boils until clean
Acetone boils until clean
Dry
Extract 3x with alcohol of choice
Evaporate to near dry, acetone flash
Recrystallize

Statement of Procedure:

1) Grind pills thoroughly. Soak for twelve hours in mineral turpentine. Alternatively soak for twelve hours in odorless mineral spirits, toluene, or xylene. Decant, discard solvent.

2) Transfer pill mass to suitable shallow bowl or evaporation dish.

3) Cover to twice its depth in non-polar solvent of choice (recommended solvent: mineral spirits). Place on heating element in a location with adequate ventilation with a fan blowing across the top of the container. Heat slowly with continuous stirring until the solvent reaches a gentle boil; adjust heat to maintain a gentle boil, with constant stirring, for five minutes. Remove from heat. Decant solvent. Use “panning” motion to separate as much solvent as possible while retaining pill mass. Alternatively, filter the solvent and pill mass through three coffee filters; retain pill mass, return to dish. Examine filtered solvent. It should be cloudy.

4) Repeat mineral spirits boils until the mineral spirits are clear when decanted. Test the clear, decanted mineral spirits by adding water; if anything precipitates out with the addition of water, repeat mineral spirits boil until the solvent is clean when decanted. Expect three boils to be necessary; dirtier pills or poor technique may require additional boils.

5) Cover the pill mass with three times its volume of dry acetone. Slowly bring to a gentle boil, with constant stirring. Boil for five minutes, allow to settle, decant. Continue with acetone boils until the decanted acetone is clean. Test for contaminants by adding water to decanted acetone and observing whether adulterants precipitate out. If so, continue acetone boils until acetone until it decants clear without adulterant precipitating with the addition of water. Expect three boils to be sufficient, depending on pill content and operator technique.

6) Allow pill mass to dry thoroughly.

7) Transfer pill mass to beaker or glass container of sufficient size to allow the addition of at least three times the pill mass’ volume of alcohol of choice. MeOH and/or denatured alcohol are recommended alcohol's. EtOH may be used if dried. Isopropyl alcohol may be used if dried. Allow pill mass to soak with agitation or stirring for twenty minutes.

8) Prepare a funnel by placing cotton balls in the neck of the funnel and fitting the funnel with three coffee filters. Decant alcohol from pill mass through three coffee filters and allow to drain into a clean glass container.

9) Return pill mass to beaker and repeat step 6, except the time for soaking should be reduced to ten minutes. Decant as before.

10) Soak pill mass a third time as in step 6, except decant after five minutes. (Save pill mass until final yield is determined to be satisfactory).

11) Place collected alcohol in evaporating dish and evaporate over very low heat, with a fan or hair dryer blowing across the surface until almost completely evaporated. Flood with dried acetone. Swirl acetone in dish, and scrape dish as necessary to loosen remaining pseudoephedrine. Decant acetone (or filter through three coffee filters.) Allow to dry.

12) Heat dried ISO alcohol to boiling. Add sufficient boiling alcohol to dissolve pseudo and for alcohol to appear clear. Filter through three coffee filters. If alcohol solution remains cloudy, filter through three coffee filters and Charmin plug. Rinse filters with small amount of fresh alcohol. Reduce volume of alcohol in evaporation dish at until first signs of crystal formation appear. Add just enough alcohol by drops to dissolve surface skin, add equal volume of dry acetone, cover with air tight lid or saran wrap, place in refrigerator.

13) Allow crystals to form; decant liquid and quickly rinse crystals with dry acetone. Add rinse acetone to remaining liquid and evaporate down to saturated alcohol, add acetone, and allow crystals to form again. Rinse these.

14) Combine crystals. Re-dissolve in boiling alcohol and repeat crystallization. Harvest final crystals.
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