* This asterisk represents any incriminating personal pronouns. “I”, “You”, etc. are people who don’t have anything to do with us.
I know what is meant by stepwise recipes. You want to know what to do first, what to do next, etc. so as to achieve product at the end. Nothing would make me happier than to provide that.
1. Put the iodine, rp and E HCl together in a 1-L flask with water and set it up for reflux.
2. Raise the temp in such a way that when it gets high enough and the rxn kicks in, adding its own heat, it doesn’t suddenly boil over. If it does act rough at first, it will settle down, but the loss of HI gas could make it too weak to effect transformation. On a website called The Hive, I think it is, or somewhere, is an apparatus called the push-and-pull apparatus, meant to answer this.
3. After 24 hours, turn off the heat. Let cool.
4. Filter out the rp. Pour the clear rxn mixture in a 2-L flask. It is going to be set up for downward distillation, for steam distillation. Filter into the 2-L flask, yeah, if you don’t break it, or slip on the floor in your stocking feet because it has plastic on it. Use cork rings to make round-bottom flasks not roll around. Clamp the neck in place on a ring stand, itself secured to remain upright when the flask gains weight. Use a funnel support. Do not assume a funnel filled to the brim with nasty liquid will just obey you and drain on in.
5. Add a previously made 50% lye solution (meaning it is cool) carefully until the thing bases over and two layers form. It spits and releases meth vapor. That is pH 10-14.
6. Steam distill into a sep funnel until no more two-phase drops come over and then some. Test the distillate if you can, when it’s water that’s all. Tap out the water and split the oil up so you don’t over-neutralize it all. Use a little diethyl ether to rinse with. Like dissolves like.
7. Neutralize to pH 7 with conc. HCl. Test with cresol red.
8. Give the neutral thing overnight to crystallize. Don’t shake it. Boil some water out if you have to, get a supersaturated solution and seed it with a tiny meth crystal if you want to see it crystallize fast.
9. Prewet the paper in a Buchner funnel/filter flask setup and pour the crystals/liquid in, turn the water aspirator pump on, do not pull air through the crystals, put the whole wet crystals, funnel in a dish and let dry. Done.