haiii!! this writeup is by ezekiel from the vespiary, link can b found here
The following is all a dream and never actually happened in real life:
Ezekiel decides to make MDA
First he takes some sassafras oil and rigs up a simple
distillation with a fridge vacuum pump. He throws away
the first stuff. When the distillate looks and smells
right, he collects 70 g. The leftovers are dark red, the
distillate is clear and smells like heaven. Oh baby!
Then he adds 7.5 g MgO and 0.7 g KOH, and heats it to a
boil for 15 min. At this time is it brown and full of
white and brown particles. After cooling, he add a bunch
of water, but the solids do not want to dissolve, and he
gets the most horrible emulsion on the planet. So he lets
it sit a while, and decants onto a vacuum filter with
qualitative paper. Lots of crap goes through and the
paper gets plugged immediately. Argh! Next time, let it
sit overnight and filter through cotton I think... He
washes the iso with water till its pale yellow, and plays
around with the solids for a while. Anyway he finally
ends up with 40 g iso. What a mess.
Then he adds 125 mL DCM and 3.75 g Na2CO3 and starts
stirring in an ice water bath. Over an hour he drips in
32 mL 35% H2O2 mixed with 72 mL 65% formic acid. He
assumed they were both v/v when calculating moles. Was he
right? Since the formic was a little more dilute than
normal, and the sirring was poor (the magnet kept jumping
around) he let it stir for 48 hrs. He then separated the
layers, both orangy, and distilled the DCM off of the
organic layer. To the residue he added 380 mL water and
started stirring. Then he added 40 mL 95% sulfuric acid.
He didn't premix cuz the heat generated boils away the
last traces of DCM. He heated the mix to 75 oC for 2 hrs.
The oil was then a dark red. He extracted with DCM,
washed with saturated bicarbonate, and distilled. When
the distillate started to get a bit orangy, he stopped.
The MDP2P was thick and yellow with the slightest green
tint. Smelled faintly like pepper and burnt wood, but
sweeter. He got 20.5 g. That's only 46.5 %, but there are
a lot of things he could have done more carefully, and
there was not one reagent grade chemical involved, so not
bad eh?
Then he decides to make some formamide. He takes 200 mL
65 % formic and adds household ammonia to pH 8 (1875 mL)
and puts this in a huge glass pot. He boils it for HOURS
until the smell changes from ammoniaish to hellish. There
was only 80 mL left and there should have been 150.
Doesn't formamide decompose below its boiling point?
Shit. Oh well, he says, the next part uses a seven-fold
excess anyway.
So Ezekiel takes his 80 mL of thick, yellow (huh?)
formamide and 20 g MDP2P and adds 10 mL water and 1 mL
glacial acetic acid. He heats this to 150 oC. After six
hours there is only 7 mL distillate. Strange. When it
separates, the oil is dark red. He extracts it with DCM,
washes with NaCl(aq) and distills off the DCM. Mmmm, red
goo.
Then he tries to mix up 27 g NaOH, 125 mL 99% IPA, and 31
mL water. This forms tree layers. White IPA on top, then
undissolved NaOH, then really hot, clear water. Oh well,
make a slurry he thinks, and adds it to the goo and
refulxes for 45 min.
At this point ol' Zeke does what I think a lot of new
bees do. He realizes that he just made X but it's in a
flask full of crap and he panics. He has never tried MDA
before and he really loses his cool and strats to goof up
a lot. So he adds some water to dilute the base, and
vacuum distills _most_ off the ethanol. (A bunch bumps
and goes out through the vac line. Ezekiel cusses
uncontrollably.) Then he extracts a few times with DCM,
and washes a few times with water. He's left with a dark
red DCM solution. What to do? He has had very bad
experiences with the gas; Logical's sulfate method sounds
appealing but probably won't work in DCM; Sunlight's
method also sounds good but the solution is REALLY dark
red; Strike and Chem Abs. say distill, but Zeke is afraid
he has such a low yield that he will lose it all to his
enormous glassware. So this is what he does.
He adds muriatic acid till the solution is pH 8. This
boils away a bunch of the DCM. This he extracts with
water. DCM layer is still dark red, water is cream
coloured. Oh baby, here's where it gets good! He rigs up
a double boiler and starts to evaporate the water layer.
Maybe there's some salt in it you think? He gives it a
taste. ARGCHHH! WOO HOO! It's not salty. Its the best
horrible taste in the WORLD, amphetamine! In about and
hour the pan in full of spaghetti-like crystals, cream
coloured. He crushed them up and weighs. 9.5 g baby!
Unless you have done something like this before, you have
NO idea how good it feels to succeed for the first time
(by a new method at least). He washed them with sub-zero,
pre-dried acetone. It turnes oh-so-slightly pink and
leaves behind a mountain of snow. Lucious. This is about
a 35 % yield, more than he ever got with Al/Hg. Ezekiel
is very very happy, even though you are all thinking your
way is better. Ezekiel knows he can improve his method
and his technique to over 50 %, which is fine in his
mind. Sassy's cheap and abundand where he lives.
Then I suddenly awoke from this dream and thought holy
shit, Ezekiel, I whish I was really you and this wasn't a
ficticious dream.
So what's the point? What's the verdict? Lessons learned?
1. Never be afraid to try new methods. It's easy to think
one is the best if it's the only one you've tried.
2. Piss on reagent grade chemicals.
3. Yield is not as important as saftey, ease, and
reliability.
4. Piss on MDMA.
5. Don't be afraid of emulsions. Better to shake good,
wait a while and get all the goodies.
6. Leuckart RULES!
7. Next time distill the formamide, do a better cleanup
of the iso, do more thorough extractions and transfers,
and be wary of the evil bumping.
8. Always be patient, careful, never panic, and save
everything.
9. Even if others diss you, try your own ideas.
10. Beg others to help you even if they know you are an
idiot and they are tired of answering your stupid
questions. How about some suggestions now?
Ooops. Sorry guyz. Ole' Zeke seems to have forgotten to
say where he dreamed of getting all this stuff without
ever even contacting a dangerous chem shop. So here goes:
sassy: essential oil shop in Ontario, no questions, no
names, pick-up ($100 per kilo)
MgO: health food store, in a bottle labelled Magnesium
Oxide Powder (cheap)
KOH: take KOH drain cleaner, boil till it gets thick,
then put it in the fridge; BANG! a zillion KOH crystals
(cheap)
NaOH: Gillet's Lye (hardware store)
filter paper: science store (crazy expensive)
DCM: distill from paint remover
sodium carbonate: bake some bicarbonate for an hour and
weigh the difference to make sure you lost the right mass
35% H2O2: hydroponics store (cheap)
65% formic acid: tanning shop or bee supply (cheap)
95% sulfuric acid: "Professional Plumber's Drain Cleaner"
at Home Deopt (cheap)
3% white ammonia: grocery store (cheap)
glacial acetic: photo store
NaCl: are you an idiot?
MgSO4: bake some epsom for an hour (cheap)
99% IPA: grocery store (cheap)
glassware, hotplate/stirrer, thermometer: science store,
surplus store, used labware store (price varies wildly)
vacuum pump: used fridge compressor (cheap)
So what do you think? No lies or exaggerations are
involed (except calling IPA ethanol in the previous post;
we're celebrating a bit here, okay?)
The following is all a dream and never actually happened in real life:
Ezekiel decides to make MDA
First he takes some sassafras oil and rigs up a simple
distillation with a fridge vacuum pump. He throws away
the first stuff. When the distillate looks and smells
right, he collects 70 g. The leftovers are dark red, the
distillate is clear and smells like heaven. Oh baby!
Then he adds 7.5 g MgO and 0.7 g KOH, and heats it to a
boil for 15 min. At this time is it brown and full of
white and brown particles. After cooling, he add a bunch
of water, but the solids do not want to dissolve, and he
gets the most horrible emulsion on the planet. So he lets
it sit a while, and decants onto a vacuum filter with
qualitative paper. Lots of crap goes through and the
paper gets plugged immediately. Argh! Next time, let it
sit overnight and filter through cotton I think... He
washes the iso with water till its pale yellow, and plays
around with the solids for a while. Anyway he finally
ends up with 40 g iso. What a mess.
Then he adds 125 mL DCM and 3.75 g Na2CO3 and starts
stirring in an ice water bath. Over an hour he drips in
32 mL 35% H2O2 mixed with 72 mL 65% formic acid. He
assumed they were both v/v when calculating moles. Was he
right? Since the formic was a little more dilute than
normal, and the sirring was poor (the magnet kept jumping
around) he let it stir for 48 hrs. He then separated the
layers, both orangy, and distilled the DCM off of the
organic layer. To the residue he added 380 mL water and
started stirring. Then he added 40 mL 95% sulfuric acid.
He didn't premix cuz the heat generated boils away the
last traces of DCM. He heated the mix to 75 oC for 2 hrs.
The oil was then a dark red. He extracted with DCM,
washed with saturated bicarbonate, and distilled. When
the distillate started to get a bit orangy, he stopped.
The MDP2P was thick and yellow with the slightest green
tint. Smelled faintly like pepper and burnt wood, but
sweeter. He got 20.5 g. That's only 46.5 %, but there are
a lot of things he could have done more carefully, and
there was not one reagent grade chemical involved, so not
bad eh?
Then he decides to make some formamide. He takes 200 mL
65 % formic and adds household ammonia to pH 8 (1875 mL)
and puts this in a huge glass pot. He boils it for HOURS
until the smell changes from ammoniaish to hellish. There
was only 80 mL left and there should have been 150.
Doesn't formamide decompose below its boiling point?
Shit. Oh well, he says, the next part uses a seven-fold
excess anyway.
So Ezekiel takes his 80 mL of thick, yellow (huh?)
formamide and 20 g MDP2P and adds 10 mL water and 1 mL
glacial acetic acid. He heats this to 150 oC. After six
hours there is only 7 mL distillate. Strange. When it
separates, the oil is dark red. He extracts it with DCM,
washes with NaCl(aq) and distills off the DCM. Mmmm, red
goo.
Then he tries to mix up 27 g NaOH, 125 mL 99% IPA, and 31
mL water. This forms tree layers. White IPA on top, then
undissolved NaOH, then really hot, clear water. Oh well,
make a slurry he thinks, and adds it to the goo and
refulxes for 45 min.
At this point ol' Zeke does what I think a lot of new
bees do. He realizes that he just made X but it's in a
flask full of crap and he panics. He has never tried MDA
before and he really loses his cool and strats to goof up
a lot. So he adds some water to dilute the base, and
vacuum distills _most_ off the ethanol. (A bunch bumps
and goes out through the vac line. Ezekiel cusses
uncontrollably.) Then he extracts a few times with DCM,
and washes a few times with water. He's left with a dark
red DCM solution. What to do? He has had very bad
experiences with the gas; Logical's sulfate method sounds
appealing but probably won't work in DCM; Sunlight's
method also sounds good but the solution is REALLY dark
red; Strike and Chem Abs. say distill, but Zeke is afraid
he has such a low yield that he will lose it all to his
enormous glassware. So this is what he does.
He adds muriatic acid till the solution is pH 8. This
boils away a bunch of the DCM. This he extracts with
water. DCM layer is still dark red, water is cream
coloured. Oh baby, here's where it gets good! He rigs up
a double boiler and starts to evaporate the water layer.
Maybe there's some salt in it you think? He gives it a
taste. ARGCHHH! WOO HOO! It's not salty. Its the best
horrible taste in the WORLD, amphetamine! In about and
hour the pan in full of spaghetti-like crystals, cream
coloured. He crushed them up and weighs. 9.5 g baby!
Unless you have done something like this before, you have
NO idea how good it feels to succeed for the first time
(by a new method at least). He washed them with sub-zero,
pre-dried acetone. It turnes oh-so-slightly pink and
leaves behind a mountain of snow. Lucious. This is about
a 35 % yield, more than he ever got with Al/Hg. Ezekiel
is very very happy, even though you are all thinking your
way is better. Ezekiel knows he can improve his method
and his technique to over 50 %, which is fine in his
mind. Sassy's cheap and abundand where he lives.
Then I suddenly awoke from this dream and thought holy
shit, Ezekiel, I whish I was really you and this wasn't a
ficticious dream.
So what's the point? What's the verdict? Lessons learned?
1. Never be afraid to try new methods. It's easy to think
one is the best if it's the only one you've tried.
2. Piss on reagent grade chemicals.
3. Yield is not as important as saftey, ease, and
reliability.
4. Piss on MDMA.
5. Don't be afraid of emulsions. Better to shake good,
wait a while and get all the goodies.
6. Leuckart RULES!
7. Next time distill the formamide, do a better cleanup
of the iso, do more thorough extractions and transfers,
and be wary of the evil bumping.
8. Always be patient, careful, never panic, and save
everything.
9. Even if others diss you, try your own ideas.
10. Beg others to help you even if they know you are an
idiot and they are tired of answering your stupid
questions. How about some suggestions now?
Ooops. Sorry guyz. Ole' Zeke seems to have forgotten to
say where he dreamed of getting all this stuff without
ever even contacting a dangerous chem shop. So here goes:
sassy: essential oil shop in Ontario, no questions, no
names, pick-up ($100 per kilo)
MgO: health food store, in a bottle labelled Magnesium
Oxide Powder (cheap)
KOH: take KOH drain cleaner, boil till it gets thick,
then put it in the fridge; BANG! a zillion KOH crystals
(cheap)
NaOH: Gillet's Lye (hardware store)
filter paper: science store (crazy expensive)
DCM: distill from paint remover
sodium carbonate: bake some bicarbonate for an hour and
weigh the difference to make sure you lost the right mass
35% H2O2: hydroponics store (cheap)
65% formic acid: tanning shop or bee supply (cheap)
95% sulfuric acid: "Professional Plumber's Drain Cleaner"
at Home Deopt (cheap)
3% white ammonia: grocery store (cheap)
glacial acetic: photo store
NaCl: are you an idiot?
MgSO4: bake some epsom for an hour (cheap)
99% IPA: grocery store (cheap)
glassware, hotplate/stirrer, thermometer: science store,
surplus store, used labware store (price varies wildly)
vacuum pump: used fridge compressor (cheap)
So what do you think? No lies or exaggerations are
involed (except calling IPA ethanol in the previous post;
we're celebrating a bit here, okay?)