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               Synthesis of DOB with NaBH4 and Al/Hg - by Iudexk
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2.84g [75mmol] NaBH4 and 1g silica gel was added to 30mL anhydr IPA and cooled
to 0C in an ice/salt bath. A solution of 4.15g [18.6mmol] 2,5-dimethoxyphenyl-
2-nitropropene in 25mL t-Bu-O-Me was then added dropwise with stirring at a rate
such that rxn temp. did not exceed 5C. Stirring was then continued at room temp.
for 6hrs. The rxn mixture was acidified by the slow addition of 50mL 32% HCl.
100mg HgCl2 was then added and dissolved. 3.011g [112mmol] aluminium foil was
then added slowly. After all Al had disappeared, rxn mixture was filtered,
tBu-O-Me/IPA evaporated, to give  red aq. layer, which was washed w/DCM, some of
the red coloring being removed, DCM extracts perfectly clear. This was then
basified, extracted w/DCM, DCM washed w/H2O, dried over MgSO4 and evaporated to
yield 1.205g 2,5-DMA as a pale yellow oil. This oil was dissolved in 7.6mL GAA,
and under sitrring 1.135g Br2 in 2.5mL GAA was added dropwise over 4mins. The
rxn mixture was left to stir for 3hrs, poured into 125mL H2O, washed w/tBu-O-Me,
basified and extracted w/DCM. The DCM was evaporated [forgot to add boiling
chip, flask overboiled, some of product lost] to give an amber oil, which was
dissolved in 75mL Et2O and gassed w/HCl [CaCl2 H2SO4] under stirring. Flask was
put in a freezer for 1hr, then filtered [filtrate pH=5.5] andd air-dried to
yield 0.69g 2,5-dimethoxy-4-bromoamphetamine hydrochloride as a white
crystalline powder.

NOTES:

1) .5g silica gel would have the same effect and not be such a bitch to
   stirring.

2) When washing the DOB.HCl/H2O w/tBu-O-Me, a huge emulsion is formed, which
   could bee avoided by the addition of 50mL or so conc. aq. NaCl, or possibly
   by washing w/Et2O instead.

3) If using Al from Al pie plates (thicker), much less molar excess (~4x) would
   bee needed.

Bioassay of product, which I am currently bioassaying as I type this, is fucking
unbelievable [nice]

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Dr Gonzo:

10g of 2,5-dimethoxy-beta-nitropropene was placed in a 300 ml beaker with
magnetic stirbar and 250 ml methanol, and stirred for a few minutes to dissolve
as much as possible. Sloooowly... 50 mg at a time... 2.2 g NaBH4 was dropped
into the sirring solution, with moderate effervescence with every addition.
Addition of all the NaBH4 took less than 30 minutes. After a little bit more
stirring, 50 ml 20% HCl was added SLOWLY - if there's any hydride left, it will
bubble vigorously. About 300 mg HgCl2 was added and allowed to dissolve (still
stirring) for a couple of minutes. Shredded kitchen aluminum foil was added,
around half a gram at a time, allowing the foil to react mostly away before the
next portion was added, in order to keep the reaction rate and temperature down.
Several grams of Al were used, and the reaction was declared finished when all
color was gone and when the chemist thought enough Al had been added. About 500
ml dH2O was added (in a new beaker), and then it was basified with 10% NaOH
until the sludge turned from solution -> gel -> granules. This was allowed to
settle, then the usual gut-wrenching Al/Hg workup was done, with multiple
dilutions, extractions, etc. When the final DCM extractions were vacuumed off,
5.5 ml of impure presumed 2,5-dimethoxyamphetamine freebase (not analyzed, just
hoped to be right) was left. Yield: approximately 60%. A drop of freebase
produced crystals with the usual ether/IPA/HCl system.

This reaction was also run on straight phenyl-beta-nitropropene, except in
absolute ethanol and not methanol. Use MeOH! EtOH yields are poor. Anyway, 16g
phenyl-beta-nitropropene was reduced to amphetamine freebase, which was then
crystallized with 93% H2SO4 in 99% IPA. Yield: 3.5-4g amphetamine sulfate.
Bioassaying the product thoroughly kicked the asses of the experimental
subjects, and also produced extreme euphoria, most likely due to the joy of
having completed a successful synthesis.

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