03-06-04 18:14
No 493441
SWIM was approached by SWIG. SWIG is a chemist and asked SWIM to invest in the material to. SWIM of course has limited experience, and is not sure if the synthesis could be successfully completed. SWIM would like to find out opinions/suggestions, or any revisions they feel would make this synthesis work. Please note that this synthesis was not in the Rhodium website, that is the reason SWIM is sceptical.....
-----------------------------
In A 3L, 3neck RBF 500ml acetonitrile water and .75g palladium(II)acetate
are
stirred until all the catalyst is dissolved.
Once the solution is clear, 13.00g p-benzoquinone and 10ml, 70% perchloric
acid
are added and the solution mixed until clear.
At this point the flask is fitted with a reflux condenser and an addition
funnel loaded with 16.22g safrole and an additional 50ml MeCN. This is
added
cautiously, maintaining a steady reflux.
TLC monitors th reaction process, and when it is determined to be complete,
the reaction mix is filtered and the products(MDP2P with traces of MDP3P
and
the aldehyde) are extracted into hexane from both the filter cake and
the
filtrate.
The hexane/ketone solution is cleaned with 20% NaOH and finally with
sat. NaCL.
The solvent is removed and the product is distilled to purity to theoretically
yield 80% or 13.8g of MDP2P.
The ketone is dissolved in 400ml dry ethanol with 45.47g titanium(IV)
isoproxide, 4.97g methylamine hydrochloride and 16.19g triethylamine
for 8- 10hrs in a sealed(but vent able through a drying tube) 3L, 3neck RBF.
A reflux condenser is then fitted in between the drying tube and the
flask, and
4.54g sodium borohydride is added carefully, maintaining the reaction temperature at 20-65 by external cooling.
TLC will monitor the reaction, and when it is complete, it will be quenced
by the addition of 300mL 1M NaOH(aq) delivered via an addition funnell fitted into
the hole through which the borohydride was added.
The mixture is then filtered and the MDMA Freebase is extracted into hexane
from both the filter cake and the filtrate.
This Organic layer is then cleaned with 1M NaOH, extracted into 10% HCL and
washed with hexane. The acidic water layer is now basified to a pH of 10 and
extracted back into hexane. A final cleaning with sat NaHco3 may or may not be
required before a sat. NaCL wash before the solvent is removed and the
product
distilled.
The pressure-equalized addition funnel is fitted into the 3L, 3neck RBF
that
has a drying tube and a hose adapter also attached. A suck back trap
is
constructed of a 3L jointed FBF with a claisen adapter and a tube adapter
in
each joint. Tubes connected the reaction vessel to the trap, and the
trap to a
glasss tube, which rests in a beaker. Conc. is placed in the addition
funnel,
and conc. HCL and NaCL in the flask. The H2S04 is dripped into the flask
where
the gas is generated. This HCL gas is then pressurized inside the reaction
vessel and is pushed out the tube to gas the MDMA Freebase in 200ml Hexane.
The commercially viable hydrochloride salt is then filtered and removed of all traces of solvent to yield~70% molecule to molecule from the principal
precursor, or 12.79g MDMA. HCL.
Startup Gear
Lab Glass(all ground glass joints in 24/40 )
3L, 3-neck round bottom flask (RBF)
300mm Graham Condenser.
3L flat bottomed flask(FBF) with sidearm.
big buchner funnel
- -box of fine filter paper to match.
fractional distillation column.
various ground glass jointed connecters.
- -vacuum distillation
- -distillation head
- -claisen adapter
- -2-ground glass jointed stopcocks
- -3-joint-to-hose adapters
- -jointed drying tube
- -some other various glassware adapters just for posterity
3L FBF w/ground glass joint
2L addition funnel
2L pressure-equalized addition funnel
5 thermometers
beakers of various sizes with watchglasses to cover some
box of capillary tubes
box of disposable pipettes with some bulbs for them.
some glass stir rods
3 6" glass stir rods
3 6" hollow glass tubes
some 4L storage bottles
Lab Gear
Mag. Stirbars to match 3l RBF, and some straight ones
Stirplate/Hotplate combo
Scale to weight 00.1g
Lab Grade Vacuum Pump of expectional quality( a reliable vacuum means consistent good yields and good quality of product ).
Digital Vacuum meter
Vacuum hosing and Acid Resistant tubing to fit the hose to joint connectors.
PH Meter
Water Aspirator
Spatulas
Lab Glass dishwashing Gear
Good Heavy Ass Table
Aquarium Pump
Lab Grade Silicone Grease
Black Light
Plastic automotive funnels of various sizes.
Box of Activated alumina TLC strips.
I fume hood which will be build out of plywood and brush less, sparkles fans,
plastic tubing etc... because SWIG gotta work with perchloric acid, and I need one
for
that.
Safrole 4l
Acetonitrile 4L
Palladium(II) acetate 10g
p-Benzoquinone 100g
70% Perchloric Acid, 2L
hexane 8L
NaOH(S) 50G
Non-iodized NaCL(Safeway)
4L ethanol
1l titanium(IV) isoproxide
50g methylamine hydrochloride
500mL triethylamine
dririte
- -white 500g
- -blue 100g
dichloromethane(or methylene chloride)
conc HCL 4L
conc H2SO4 4L
NaHCO3(s)(safeway)In A 3L, 3neck RBF 500ml acetonitrile water and .75g
palladium
(II)acetate are stirred until all the catalyst is dissolved.
Once the solution is clear, 13.00g p-benzoquinone and 10ml, 70% perchloric
acid
are added and the solution mixed until clear.
At this point the flask is fitted with a reflux condenser and an addition
funnel loaded with 16.22g safrole and an additional 50ml MeCN. This is
added
cautiously, maintaining a steady reflux.
TLC monitors th reaction process, and when it is determined to be complete,
the reaction mix is filtered and the products(MDP2P with traces of MDP3P
and
the aldehyde) are extracted into hexane from both the filter cake and
the
filtrate.
The hexane/ketone solution is cleaned with 20% NaOH and finally with
sat. NaCL.
The solvent is removed and the product is distilled to purity to theoretically
yield 80% or 13.8g of MDP2P.
The ketone is dissolved in 400ml dry ethanol with 45.47g titanium(IV)
isoproxide, 4.97g methylamine hydrochloride and 16.19g triethylamine
for 8-
10hrs in a sealed(but vent able through a drying tube) 3L, 3neck RBF.
A reflux condenser is then fitted in between the drying tube and the
flask, and
4.54g sodium borohydride is added carefully, maintaining the reaction
temperature at 20-65 by external cooling.
TLC will monitor the reaction, and when it is complete, it will be quenced
by
the addition of 300mL 1M NaOH(aq) delivered via an addition funnell fitted
into
the hole through which the borohydriede was added.
The mixture is then filtered and the MDMA Freebase is extracted into
hexane
from both the filter cake and the filtrate.
This Organic layer is then cleaned with 1M NaOH, extracted into 10% HCL
and
washed with hexane. The acidic water layer is now basified to a pH of
10 and
extracted back into hexane. A final cleaning with sat NaHco3 may or may
not be
required before a sat. NaCL wash before the solvent is removed and the
product
distilled.
The pressure-equalized addition funnel is fitted into the 3L, 3neck RBF
that
has a drying tube and a hose adapter also attached. A suck back trap
is
constructed of a 3L jointed FBF with a claisen adapter and a tube adapter
in
each joint. Tubes connected the reaction vessel to the trap, and the
trap to a
glasss tube, which rests in a beaker. Conc. is placed in the addition
funnel,
and conc. HCL and NaCL in the flask. The H2S04 is dripped into the flask
where
the gas is generated. This HCL gas is then pressurized inside the reaction
vessel and is pushed out the tube to gas the MDMA Freebase in 200ml Hexane.
The
commercially viable hydrochloride salt is then filtered and removed of
all
traces of solvent to yield~70% molecule to molecule from the principal
precursor, or 12.79g MDMA. HCL.
Startup Gear
Lab Glass(all ground glass joints in 24/40
3L, 3-neck round bottom flask (RBF)
300mm Graham Condenser.
3L flat bottomed flask(FBF) with sidearm.
big buchner funnel
- -box of fine filter paper to match.
fractional distillation column.
various ground glass jointed connecters.
- -vacuum distillation
- -distillation head
- -claisen adapter
- -2-ground glass jointed stopcocks
- -3-joint-to-hose adapters
- -jointed drying tube
- -some other various glassware adapters just for posterity
3L FBF w/ground glass joint
2L addition funnel
2L pressure-equalized addition funnel
5 thermometers
beakers of various sizes with watchglasses to cover some
box of capillary tubes
box of disposable pipettes with some bulbs for them.
some glass stir rods
3 6" glass stir rods
3 6" hollow glass tubes
some 4L storage bottles
Lab Gear
Mag. Stirbars to match 3l RBF, and some straight ones
Stirplate/Hotplate combo
Scale to weight 00.1g
Lab Grade Vacuum Pump of expectional quality( a reliable vacuum means
consistent good yields and good quality of product ).
Digital Vacuum meter
Vacuum hosing and Acid Resistant tubing to fit the hose to joint connectors.
PH Meter
Water Aspirator
Spatulas
Lab Glass dishwashing Gear
Good Heavy Ass Table
Aquarium Pump
Lab Grade Silicone Grease
Black Light
Plastic automotive funnels of various sizes.
Box of Activated alumina TLC strips.
I wanna build a fume hood out of plywood and brush less, sparkles fans,
plastic
tubing etc... because swig gotta work with perchloric acid, and SWIG need one
for
that.
Safrole 4l
Acetonitrile 4L
Palladium(II) acetate 10g
p-Benzoquinone 100g
70% Perchloric Acid, 2L
hexane 8L
NaOH(S) 50G
Non-iodized NaCL(Safeway)
4L ethanol
1l titanium(IV) isoproxide
50g methylamine hydrochloride
500mL triethylamine
dririte
- -white 500g
- -blue 100g
dichloromethane(or methylene chloride)
conc HCL 4L
conc H2SO4 4L
NaHCO3(s)(safeway)
------------------
So basically SWIM is looking for advice/input from any bees that can review the proposal, and advice SWIM if it can be successfully produce MDMA HCL. Any revisions/variations that fellow bees would like to suggest will be definitely appreciated.
(Pioneer Researcher)
03-07-04 13:58
No 493587
The first part is a variation of the benzo wacker that supposedly is faster. 0.75 gr of Pd acetate is a waste, about 0.2 will be enough for 16.2 gr of safrol.
(Old P2P Cook)
03-08-04 01:09
No 493657
Be very carefull with 70% perchloric acid. If you don't you might burn down your lab or have a nice explosion.
All those moments will be lost in time, like tears in rain.
(Hive Bee)
03-08-04 19:26
No 493781
So, do you bees recommend doing the benzo wacker instead of the proposed variation?
Also could something else be substituted for perchloric acid?
(Old P2P Cook)
03-10-04 03:59
No 494088
Stick with the Benzoquinone Wacker. The perchloric acid seems an unnecessary and dangerous complication.
All those moments will be lost in time, like tears in rain.
(Hive Bee)
03-10-04 20:59
No 494246
IMHO go with the benzo wacker,and LabTop's Borohydride reduction...fewer different and easier supplies to get means less risk.
They have never failed P:always get 115 to 120g ketone from 180g saf,and 950 to 980g freebase from 1000g ketone.
KIS