Why on Earth do it the hard way?
65% Formic acid: tanning shops or bee-keepers supply shops (cheap btw).
Dump into this 65% formic acid 250 gram/liter zeolites type 3A, aka molecular sieves, mesh 4-8, swirl occasionally while let stand a few hours, decant and repeat with fresh Type 3A molecular sieves , until you have reached the density of 90% formic acid, needed in the next procedure. (Check d20°C with balance and 100ml exact measureing flask)
Yeah, fuck, what's the d20°C of 90% formic acid? Look it up : ?,?? g/ml!
Formic acid 96%, HCO2H:
mp=8.2-8.4° , bp=100-101° , d=1.220
Check on the label if "they" included any other shit than water! Then you have to distill or precipitate that shit out first.
'I ever got a can of the 4-8 mesh, little balls of rock about 1/8" = 3 mm, diameter. They absorb about 20% of their weight of water over the course of a few hours. Not expensive either : US$ 2.05 a pound in 10 lb quantities, and reusable indefinitely. You drive off the water under a broiler for an hour.
Take f.e. a liter of 95% ethanol, throw in 250g of the stuff, swirl occasionally, filter out the next day through a strainer, and voila! Anhydrous 99%++ ethanol pure; anhydrous that is, with less than 1% water content. The purest ethanol that can be produced by ordinary distillation is only 95.6% pure, the rest being water. More common for home distillation is 170-190 proof -- 85-95% pure.'
http://www.thomasregister.com/olc/adcoa/molecula.htm
This gives quite some info on molecular sieves!
Ehh, what more.., ahhh, Formamide! Make it in situ :
Ref:
J. Am. Chem. Soc. 75, 921-925 (1953)
(
https://www.thevespiary.org/rhodium/Rhodium/pdf/2-meo-methamphetamine.pdf)
The most simplistic Leuckart Reaction :
Take a three-necked, 2 Liter RB-flask, fit it with :
A dropping funnel, a thermometer reaching to 1 cm from the bottom, a Friedrich condenser arranged for downward distillation (so not reflux), and a magnetic stirbar .
Add 315 ml of 28% aqueous ammonia (NH4OH) to the 2 L RB-flask.
Stir this solution and add dropwise 264 ml of 90% formic acid.
Then remove the stirbar and heat the solution gradually over a 2 to 3 hour period to 160°C, the temperature being regulated so that fairly rapid distillation takes place. (throw distillate away).
........
==>>After cooling back to 110°C, 164 g. (1.0 mol) of o-methoxyphenylacetone is added and the mixture heated at 160-170°C for 5 hours. (1.0 mol of MDP2P = 178.8 g, so use that instead!)
At the end of the first 2 hours period, the upper layer of the distillate is returned to the reaction flask.
After standing overnight the homogenous solution is heated 2 hours more.<<==
........
It is then cooled back to 70°C , 360 ml of concentrated hydrochloric acid (31-33%) is added dropwise and the mixture heated for 6 hours under reflux and allowed to stand overnight.
The suspension is diluted with 600 ml of water and extracted several times with benzene (or toluene, or whatever suites you).
The aqueous layer is basified, extracted with benzene ( or etc.) and the residue from the benzene distilled under an atmosphere of nitrogen; b.p. 118-122 deg C at 11mm, yield 95 g. (58%).
(This yield is for o-methoxyphenylacetone, not for MDP2P! No need for nitrogen atmosphere either!
You will find out yourself what the yield is for MDA...)According to rumors in the Hive corridors, the procedure between the ==>> <<== could be done at a more moderate temperature, say 135 to 140°C, where a just noticeable CO2 bubbling in the reactionmix is the threshhold for the max temperature allowed, and for an extended period of up to 3 days. This is said to increase yields into the 70% figures... LT/
Ahh, can't resist, an Extra:
Separating Ethanol From Water Via Differential Miscibility.The differential miscibility of castor oil in ethanol and water can be exploited to separate ethanol from water.
Burning the separated ethanol would
produce more energy than would be consumed in the separation process. Very energy
saving!In contrast, the separation of a small amount of ethanol (actually an ethanol/water solution poor in ethanol) from water by the conventional process of distillation
requires more energy than can be produced by burning the resulting distillate. Very energy
consuming!Castor oil would be added to an ethanol/water solution. The ethanol would mix freely with castor oil, which is insoluble in water. The resulting ethanol/castor-oil phase, which would contain less than 1 percent water, would collect as the top layer, the bottom layer being the remainder of the ethanol/water solution somewhat depleted in ethanol. Heating this two-layer mixture to a temperature slightly below the boiling temperature of ethanol (78.5 deg C) would cause the partial pressure of ethanol above the top layer to be much greater than the partial pressure of either castor oil or water. This vapor-phase ethanol could be condensed in a relatively pure state.
Although heating an isolated ethanol/water solution like that in the bottom layer would normally raise the vapor pressure of both ethanol and water above the solution, this would not be the case in the presence of the top castor-oil/ethanol layer for the following reasons: The amount of water that could dissolve in the top castor-oil/ethanol layer would increase only slightly upon heating. On the other hand, ethanol could readily cross the interface between the two layers and enter the top layer. As long as the total mix was kept at a temperature below the boiling temperature of ethanol (thereby preventing agitation of the layers by boiling), the diffusion of water through the castor-oil/ethanol phase would be inhibited.
In an alternative version of this concept, the upper castor-oil/ethanol layer would be skimmed off and heated to obtain the ethanol. Once the ethanol was driven off, the castor oil could be returned to an ethanol/water solution to dissolve more ethanol to repeat the process. This concept could readily lend itself to a continuous process. Substances other than castor oil (one of its components perhaps, or another substance) could be used in this process or to extract other compounds from other mixtures by using this upper-of-two-phases vaporization technique.
Do not start a factory based on this, I will start that first,
.
WISDOMwillWIN