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Have a really odd question.
Don't know if anyone can help or not, but hope so.
Don't know if anyone can help or not, but hope so.
Any chemists out there?
- Thread starter LattimerII
- Start date
chemist or illegal drug manufacture
XTC SYNTHESIS: (from MDA) A solution of 6.55 g of 3,4-methylenedioxyamphetamine
(MDA) as the free base and 2.8 mL formic acid in 150 mL benzene was held at
reflux under a Dean Stark trap until no further H2O was generated (about 20 h
was sufficient, and 1.4 mL H2O was collected). Removal of the solvent gave an
8.8 g of an amber oil which was dissolved in 100 mL CH2Cl2, washed first with
dilute HCl, then with dilute NaOH, and finally once again with dilute acid. The
solvent was removed under vacuum giving 7.7 g of an amber oil that, on standing,
formed crystals of N-formyl-3,4-methylenedioxyamphetamine. An alternate process
for the synthesis of this amide involved holding at reflux for 16 h a solution
of 10 g of MDA as the free base in 20 mL fresh ethyl formate. Removal of the
volatiles yielded an oil that set up to white crystals, weighing 7.8 g.
A solution of 7.7 g N-formyl-3,4-methylenedioxyamphetamine in 25 mL anhydrous
THF was added dropwise to a well stirred and refluxing solution of 7.4 g LAH in
600 mL anhydrous THF under an inert atmosphere. The reaction mixture was held at
reflux for 4 days. After being brought to room temperature, the excess hydride
was destroyed with 7.4 mL H2O in an equal volume of THF, followed by 7.4 mL of
15% NaOH and then another 22 mL H2O. The solids were removed by filtration, and
the filter cake washed with additional THF. The combined filtrate and washes
were stripped of solvent under vacuum, and the residue dissolved in 200 mL
CH2Cl2. This solution was extracted with 3x100 mL dilute HCl, and these extracts
pooled and made basic with 25% NaOH. Extraction with 3x75 mL CH2Cl2 removed the
product, and the pooled extracts were stripped of solvent under vacuum. There
was obtained 6.5 g of a nearly white residue which was distilled at 100-110 ° C
at 0.4 mm/Hg to give 5.0 g of a colorless oil. This was dissolved in 25 mL IPA,
neutralized with concentrated HCl, followed by the addition of sufficient
anhydrous Et2O to produce a lasting turbidity. On continued stirring, there was
the deposition of fine white crystals of 3,4-methylenedioxy-N-methylamphetamine
hydrochloride (MDMA) which were removed by filtration, washed with Et2O, and air
dried, giving a final weight of 4.8 g.
(from 3,4-methylenedioxyphenylacetone) This key intermediate to all of the
MD-series can be made from either isosafrole, or from piperonal via
1-(3,4-methylenedioxyphenyl)-2-nitropropene. To a well stirred solution of 34 g
of 30% hydrogen peroxide in 150 g 80% formic acid there was added, dropwise, a
solution of 32.4 g isosafrole in 120 mL acetone at a rate that kept the reaction
mixture from exceeding 40 ° C. This required a bit over 1 h, and external
cooling was used as necessary. Stirring was continued for 16 h, and care was
taken that the slow exothermic reaction did not cause excess heating. An
external bath with running water worked well. During this time the solution
progressed from an orange color to a deep red. All volatile components were
removed under vacuum which yielded some 60 g of a very deep red residue. This
was dissolved in 60 mL of MeOH, treated with 360 mL of 15% H2SO4, and heated for
3 h on the steam bath. After cooling, the reaction mixture was extracted with
3x75 mL Et2O, the pooled extracts washed first with H2O and then with dilute
NaOH, and the solvent removed under vacuum The residue was distilled (at 2.0
mm/108-112 ° C, or at about 160 ° C at the water pump) to provide 20.6 g of
3,4-methylenedioxyphenylacetone as a pale yellow oil. The oxime (from
hydroxylamine) had a mp of 85-88 ° C. The semicarbazone had a mp of 162-163 ° C.
An alternate synthesis of 3,4-methylenedioxyphenylacetone starts originally from
piperonal. A suspension of 32 g electrolytic iron in 140 mL glacial acetic acid
was gradually warmed on the steam bath. When quite hot but not yet with any
white salts apparent, there was added, a bit at a time, a solution of 10.0 g of
1-(3,4-methylenedioxyphenyl)-2-nitropropene in 75 mL acetic acid (see the
synthesis of MDA for the preparation of this nitrostyrene intermediate from
piperonal and nitroethane). This addition was conducted at a rate that permitted
a vigorous reaction free from excessive frothing. The orange color of the
reaction mixture became very reddish with the formation of white salts and a
dark crust. After the addition was complete, the heating was continued for an
additional 1.5 h during which time the body of the reaction mixture became quite
white with the product appeared as a black oil climbing the sides of the beaker.
This mixture was added to 2 L H2O, extracted with 3x100 mL CH2Cl2, and the
pooled extracts washed with several portions of dilute NaOH. After the removal
of the solvent under vacuum, the residue was distilled at reduced pressure (see
above) to provide 8.0 g of 3,4-methylenedioxyphenylacetone as a pale yellow oil.
To 40 g of thin aluminum foil cut in 1 inch squares (in a 2 L wide mouth
Erlenmeyer flask) there was added 1400 mL H2O containing 1 g mercuric chloride.
Amalgamation was allowed to proceed until there was the evolution of fine
bubbles, the formation of a light grey precipitate, and the appearance of
occasional silvery spots on the surface of the aluminum. This takes between 15
and 30 min depending on the freshness of the surfaces, the temperature of the
H2O, and the thickness of the aluminum foil. (Aluminum foil thickness varies
from country to country.) The H2O was removed by decantation, and the aluminum
was washed with 2x1400 mL of fresh H2O. The residual H2O from the final washing
was removed as thoroughly as possible by shaking, and there was added, in
succession and with swirling, 60 g methylamine hydrochloride dissolved in 60 mL
warm H2O, 180 mL IPA, 145 mL 25% NaOH, 53 g 3,4-methylenedioxyphenylacetone, and
finally 350 mL IPA. If the available form of methylamine is the aqueous solution
of the free base, the following sequence can be substituted: add, in succession,
76 mL 40% aqueous methylamine, 180 mL IPA, a suspension of 50 g NaCl in 140 mL
H2O that contains 25 mL 25% NaOH, 53 g 3,4-methylenedioxyphenylacetone, and
finally 350 mL IPA. The exothermic reaction was kept below 60 ° C with
occasional immersion into cold water and, when it was thermally stable, it was
allowed to stand until it had returned to room temperature with all the
insolubles settled to the bottom as a grey sludge. The clear yellow overhead was
decanted and the sludge removed by filtration and washed with MeOH. The combined
decantation, mother liquors and washes, were stripped of solvent under vacuum,
the residue suspended in 2400 ml of H2O, and sufficient HCl added to make the
phase distinctly acidic. This was then washed with 3x75 mL CH2Cl2, made basic
with 25% NaOH, and extracted with 3x100 mL of CH2Cl2. After removal of the
solvent from the combined extracts, there remained 55 g of an amber oil which
was distilled at 100-110 ° C at 0.4 mm/Hg producing 41 g of an off-white liquid.
This was dissolved in 200 mL IPA, neutralized with about 17 mL of concentrated
HCl, and then treated with 400 mL anhydrous Et2O. After filtering off the white
crystals, washing with an IPA/Et2O mixture, (2:1), with Et2O, and final air
drying, there was obtained 42.0 g of 3,4-methylenedioxy-N-methylamphetamine
(MDMA) as a fine white crystal. The actual form that the final salt takes
depends upon the temperature and concentration at the moment of the initial
crystallization. It can be anhydrous, or it can be any of several hydrated
forms. Only the anhydrous form has a sharp mp; the published reports describe
all possible one degree melting point values over the range from 148-153 ° C.
The variously hydrated polymorphs have distinct infrared spectra, but have broad
mps that depend on the rate of heating.
DOSAGE: 80 - 150 mg.
DURATION: 4 - 6 h.
XTC SYNTHESIS: (from MDA) A solution of 6.55 g of 3,4-methylenedioxyamphetamine
(MDA) as the free base and 2.8 mL formic acid in 150 mL benzene was held at
reflux under a Dean Stark trap until no further H2O was generated (about 20 h
was sufficient, and 1.4 mL H2O was collected). Removal of the solvent gave an
8.8 g of an amber oil which was dissolved in 100 mL CH2Cl2, washed first with
dilute HCl, then with dilute NaOH, and finally once again with dilute acid. The
solvent was removed under vacuum giving 7.7 g of an amber oil that, on standing,
formed crystals of N-formyl-3,4-methylenedioxyamphetamine. An alternate process
for the synthesis of this amide involved holding at reflux for 16 h a solution
of 10 g of MDA as the free base in 20 mL fresh ethyl formate. Removal of the
volatiles yielded an oil that set up to white crystals, weighing 7.8 g.
A solution of 7.7 g N-formyl-3,4-methylenedioxyamphetamine in 25 mL anhydrous
THF was added dropwise to a well stirred and refluxing solution of 7.4 g LAH in
600 mL anhydrous THF under an inert atmosphere. The reaction mixture was held at
reflux for 4 days. After being brought to room temperature, the excess hydride
was destroyed with 7.4 mL H2O in an equal volume of THF, followed by 7.4 mL of
15% NaOH and then another 22 mL H2O. The solids were removed by filtration, and
the filter cake washed with additional THF. The combined filtrate and washes
were stripped of solvent under vacuum, and the residue dissolved in 200 mL
CH2Cl2. This solution was extracted with 3x100 mL dilute HCl, and these extracts
pooled and made basic with 25% NaOH. Extraction with 3x75 mL CH2Cl2 removed the
product, and the pooled extracts were stripped of solvent under vacuum. There
was obtained 6.5 g of a nearly white residue which was distilled at 100-110 ° C
at 0.4 mm/Hg to give 5.0 g of a colorless oil. This was dissolved in 25 mL IPA,
neutralized with concentrated HCl, followed by the addition of sufficient
anhydrous Et2O to produce a lasting turbidity. On continued stirring, there was
the deposition of fine white crystals of 3,4-methylenedioxy-N-methylamphetamine
hydrochloride (MDMA) which were removed by filtration, washed with Et2O, and air
dried, giving a final weight of 4.8 g.
(from 3,4-methylenedioxyphenylacetone) This key intermediate to all of the
MD-series can be made from either isosafrole, or from piperonal via
1-(3,4-methylenedioxyphenyl)-2-nitropropene. To a well stirred solution of 34 g
of 30% hydrogen peroxide in 150 g 80% formic acid there was added, dropwise, a
solution of 32.4 g isosafrole in 120 mL acetone at a rate that kept the reaction
mixture from exceeding 40 ° C. This required a bit over 1 h, and external
cooling was used as necessary. Stirring was continued for 16 h, and care was
taken that the slow exothermic reaction did not cause excess heating. An
external bath with running water worked well. During this time the solution
progressed from an orange color to a deep red. All volatile components were
removed under vacuum which yielded some 60 g of a very deep red residue. This
was dissolved in 60 mL of MeOH, treated with 360 mL of 15% H2SO4, and heated for
3 h on the steam bath. After cooling, the reaction mixture was extracted with
3x75 mL Et2O, the pooled extracts washed first with H2O and then with dilute
NaOH, and the solvent removed under vacuum The residue was distilled (at 2.0
mm/108-112 ° C, or at about 160 ° C at the water pump) to provide 20.6 g of
3,4-methylenedioxyphenylacetone as a pale yellow oil. The oxime (from
hydroxylamine) had a mp of 85-88 ° C. The semicarbazone had a mp of 162-163 ° C.
An alternate synthesis of 3,4-methylenedioxyphenylacetone starts originally from
piperonal. A suspension of 32 g electrolytic iron in 140 mL glacial acetic acid
was gradually warmed on the steam bath. When quite hot but not yet with any
white salts apparent, there was added, a bit at a time, a solution of 10.0 g of
1-(3,4-methylenedioxyphenyl)-2-nitropropene in 75 mL acetic acid (see the
synthesis of MDA for the preparation of this nitrostyrene intermediate from
piperonal and nitroethane). This addition was conducted at a rate that permitted
a vigorous reaction free from excessive frothing. The orange color of the
reaction mixture became very reddish with the formation of white salts and a
dark crust. After the addition was complete, the heating was continued for an
additional 1.5 h during which time the body of the reaction mixture became quite
white with the product appeared as a black oil climbing the sides of the beaker.
This mixture was added to 2 L H2O, extracted with 3x100 mL CH2Cl2, and the
pooled extracts washed with several portions of dilute NaOH. After the removal
of the solvent under vacuum, the residue was distilled at reduced pressure (see
above) to provide 8.0 g of 3,4-methylenedioxyphenylacetone as a pale yellow oil.
To 40 g of thin aluminum foil cut in 1 inch squares (in a 2 L wide mouth
Erlenmeyer flask) there was added 1400 mL H2O containing 1 g mercuric chloride.
Amalgamation was allowed to proceed until there was the evolution of fine
bubbles, the formation of a light grey precipitate, and the appearance of
occasional silvery spots on the surface of the aluminum. This takes between 15
and 30 min depending on the freshness of the surfaces, the temperature of the
H2O, and the thickness of the aluminum foil. (Aluminum foil thickness varies
from country to country.) The H2O was removed by decantation, and the aluminum
was washed with 2x1400 mL of fresh H2O. The residual H2O from the final washing
was removed as thoroughly as possible by shaking, and there was added, in
succession and with swirling, 60 g methylamine hydrochloride dissolved in 60 mL
warm H2O, 180 mL IPA, 145 mL 25% NaOH, 53 g 3,4-methylenedioxyphenylacetone, and
finally 350 mL IPA. If the available form of methylamine is the aqueous solution
of the free base, the following sequence can be substituted: add, in succession,
76 mL 40% aqueous methylamine, 180 mL IPA, a suspension of 50 g NaCl in 140 mL
H2O that contains 25 mL 25% NaOH, 53 g 3,4-methylenedioxyphenylacetone, and
finally 350 mL IPA. The exothermic reaction was kept below 60 ° C with
occasional immersion into cold water and, when it was thermally stable, it was
allowed to stand until it had returned to room temperature with all the
insolubles settled to the bottom as a grey sludge. The clear yellow overhead was
decanted and the sludge removed by filtration and washed with MeOH. The combined
decantation, mother liquors and washes, were stripped of solvent under vacuum,
the residue suspended in 2400 ml of H2O, and sufficient HCl added to make the
phase distinctly acidic. This was then washed with 3x75 mL CH2Cl2, made basic
with 25% NaOH, and extracted with 3x100 mL of CH2Cl2. After removal of the
solvent from the combined extracts, there remained 55 g of an amber oil which
was distilled at 100-110 ° C at 0.4 mm/Hg producing 41 g of an off-white liquid.
This was dissolved in 200 mL IPA, neutralized with about 17 mL of concentrated
HCl, and then treated with 400 mL anhydrous Et2O. After filtering off the white
crystals, washing with an IPA/Et2O mixture, (2:1), with Et2O, and final air
drying, there was obtained 42.0 g of 3,4-methylenedioxy-N-methylamphetamine
(MDMA) as a fine white crystal. The actual form that the final salt takes
depends upon the temperature and concentration at the moment of the initial
crystallization. It can be anhydrous, or it can be any of several hydrated
forms. Only the anhydrous form has a sharp mp; the published reports describe
all possible one degree melting point values over the range from 148-153 ° C.
The variously hydrated polymorphs have distinct infrared spectra, but have broad
mps that depend on the rate of heating.
DOSAGE: 80 - 150 mg.
DURATION: 4 - 6 h.
LattimerII
New member
Damn!
I meant more along the lines of college chemistry prof. I've got a wierd inquiry for a legit chemist (not to say underground chemists can't be good at what they do
). We've got a wide variety of people on elite, so I figured I'd give it a shot. Thanks for the info though.
I meant more along the lines of college chemistry prof. I've got a wierd inquiry for a legit chemist (not to say underground chemists can't be good at what they do
). We've got a wide variety of people on elite, so I figured I'd give it a shot. Thanks for the info though.Similar threads
