Synthesis of DOB by Phikshun2
2,5-dimethoxyphenyl-2-nitropropene
10.0g of 2,5 dimethoxybenzaldehyde was dissolved in 50mL of GAA, and 6.8g of nitroethane was added. I dreamed I got both from a photochemical supplier with relative ease. 4.0g of ammonium acetate, that had been stored for weeks over Calcium Chloride (i.e. quite anhydrous), was added and the flask swirled until everything dissolved. This mixture was heated over a pot of boiling water, with heavy duty foil surrounding the flask and top of pot, to keep steam in. It was left for nearly 3 hours, upon which time it had a cherry red colour, and was allowed to cool. After cooling, solvent was stripped off under aspirator vacuum and about 100mL of dH2O was added. The mixture was then extracted with TCE (tetrachloroethylene, brake degreaser, don't ask), and the TCE distilled off under vacuum to afford 12.4g of impure nitropropene, which was recrystallized in 80mL methanol to ~10g, and was recrystallized again from 75mL methanol to a weight of 8.4g. I have no idea why Shulgin only got 6.7g in his 2,5-DMA synth.
2,5-dimethoxyamphetamine
Prepared Urushibara catalyst using instructions from
https://www.thevespiary.org/rhodium/Rhodium/chemistry/tmp2np-red.html
. Had to use a cleaned out 4L milk jug instead of a 4L beaker, and I used nuggetized generic Al foil, but otherwise the same method. Activated 15g of the aforementioned catalyst in 580mL of 40% GAA, with 130g of NaCl dissolved, at 70 deg C for a little over 7 mins. Rinsed with 60 deg C dH2O and washed with IPA, then placed in a 500mL erlenmeyer with 375mL of anhydrous IPA, and 6.7g of the long orange crystalline needles of nitropropene prepped in the previous step. The yellow-orange tint completely leaves the solution in about an hour. For stirring, SWIM used a 12V computer fan, with the blades cut off and a glass stir rod (slightly bent on the end) fastened on with a rubber stopper and some crazy glue. This was attached with a 12V supply with a variable resistor in place to control speed. Worked famously, and totally quiet, which is good, because this dream took place in a small apt. 15g of Al foil prepped in the same fashion as used to precipitate catalyst, is added gram wise, followed by the addition of 3ml 31.45% HCl (HW store grade). This took about 2.5 hours. The flask got quite warm near the middle of the reaction, but never achieves reflux. After Al stops reacting, and H2 is no longer bubbling, 150ml of IPA is added, and then the reaction is basified with 50% NaOH sol. After bubbling subsides, nice yellowish alcoholic layer settled out on top. This was decanted, and concentrated at aspirator vacuum. The remaining AlO sludge is extracted with xylene, and the xylene is added to the other extracts. This was washed once with Brine, and once with dH2O, then dH2O is added, and triturated to a pH of 4. Aqueous extract is kept, basified with NaOH solution and extracted with DCM. DCM is evaporated overnight to provide ~3ml of orangish brown oil. Further A/B extractions of the xylene proved not to contain any more DMA.
4-bromo-2,5-dimethoxyamphetamine
The crude DMA, which weighed 2.1g, and 15ml GAA was placed in a 50ml RBF with a claisen adaptor attached, a condenser, then a gas inlet adaptor, which was hooked to a tube leading outside. Upon the claisen was placed a 125ml addition funnel. Into the funnel was added 2g elemental bromine (I chilled it first in the fridge, still reeked) in 5ml GAA. This was dripped in over a 5 minute period with magnetic stirring, and was left for about 4 hours. This mixture was then added to 200mL dH20, and washed with 3x50mL portions of xylene. This was basified with a 25% NaOH solution, then extracted with 100mL and then 50mL of DCM. Upon evaporation of the solvent, about 3-4ml of a pale brown oil was recovered, which crystallized on standing overnight. To this was added sufficient IPA to dissolve, and it was triturated dropwise with 31% HCl until a pH of 4 was obtained. IPA was distilled off until about 20mL remained, then cold acetone was added to crash out the crystals. Solution was vacuum filtered, and the resulting off-white crystals where recrystallized in IPA to afford 1.25g of perfectly white, fine, powder of DOB.HCl. This worked out to about 415 hits, at 3mg a piece. Personally, I really don’t enjoy DOB that much, but it makes acid look like kids stuff. My roommate loves the stuff though...
P.S. I never claimed this was anything revolutionary, but it's my first dream. Thanks to everyone at the hive who make dreams great