MethCat failure

[jtryptamine]

Swij was bored and decided to try a cat rxn just for shits and giggles. He dissloved 10g pseudoephedrine in 25mL acetone and Put beaker in a ice salt bath.

 He then mixed 12.5mL of water w/ 5mL 96% H ₂SO₄then added 3.3g CrO₃.after cooling
He then added the CrO₃ solution dropwise to the pfed solution in the ice/salt bath w/ magnetic stirring. The addition took 15min.

  The stirring was continued for a reaction time of 3.5 hours. He Then poured the solution in ten volumes of water and a 20% solution of NaOH in water was added until strongly alkaline, then the solution was extracted using two 25mL portions of toluene. The extractions were colored PINK.
The toluene was washed with 50mL water which did not remove the pink hue.

 The toluene was poured of and let sit for 1 hour, then poured into a clean beaker. He proceeded to bubble dry HCl through it, which then turned the solution light blue. No crystals precipitated out, not even pfed. He cannot figure out what happened, and why the solution changed colors. The solution has now been sitting around for another hour and is taking on a urine color. The pfed was very clean (nice long crystals) and dry so the pink wasn't from the pills. Any guesses of what happened?

[amalgum]

Probably let it sit to long, and it got over oxidised into useless garbage.  SWIM has attempted methcathinone synths in the past before for shits and giggles as well.  However, SWIM just mixed a saturated solution of pfed HCl in H2O with chromic acid solution, and only let it sit for an hour or so (not 3+!!!) before it turned dark greenish, indicating completion of desired rxn.  SWIM always failed however (only tried twice) because pill gaks mixed with the power of the chromic acid acting on them was hell on extraction, and nothing could really be worked out of it.  SWIM never tried to do anything more than a final a/b, which horrible, and being that it was only methcathinone SWIM always abandoned the shit and never went beyond that.  SWIM does know the oxidation itself worked somewhat properly, as the pistacio smell could be detected when based, and acidified solutions containing the suspected drug smelled strongly of cherries, a sure indication that methcathinone was present somewhere in there.

[alphacentauri]

I think adding sulphuric before the oxidizer is a mistake, because the alcoholic function of ephedrine is not inert in a strong acidic medium.
The precursor, then, should be as pure as possible. You can have the evidence of its purity watching the cristallization shapes at the bottom of your beaker when you do the final evaporation. These cristal shapes are very typical.
The oxidation must be performed "at room temperature". Now, in the hot subtropical summer, I put the flask with the dichromate in the fridge the night before. I add sulphuric only AFTER the dichromate and SLOWLY under stirring. When the solution becomes dark and the meniscus is green the reaction is almost complete. If you work properly the reaction doesn't proceed further the formation of the ketone. If you heat it up immediately you'll have the formation of benzoic acid.
You must add the NaOH (or KOH) COLD taken from the fridge only while stirring, little by little, till you see the formation of "milk 'n coffee". At that moment check the pH at every TINY addition of base. When the free base is complete shake in the sep funnel with chloroform, or toluene, or perchloroethylene (3 extractions), then wash it 3 times with distilled water till the free base-solvent layer is light grey, then make the hydrochloride directly in the sep funnel adding first the water with HCl (10-15 drops every expcted gram), after shaking the indicator reads basic. Then you correct to 6-7 adding 4-5 drops of acid, new reading, new corrction, till you reach the right  pH. Then concentrate the water till you see the formation of a light greenish cloud. Now filter it and finish the evaporation at moderate temperature. If you have worked properly you'll see the formation of the same typical crystallization pattern of ephedrine, but that is methcathinone, believe me. In the end, add acetone, let it stand a while, remove the acetone carefully with a syringe, then let the last acetone evaporate at room temperature or VERY MODERATE heat. Scrape with a spatula and....have a good day. The powder you'll get in this way is white shiny and the small crystals are needle shaped. Have you ever tried to drink a tea of salvia divinorum while on cat?