02-02-03 08:45
No 403641
I am writing a story about a man named Chuck. Chuck isn't at his lab. So, chuck finds himself in a situation that demands creativity.
"Take 294 grams of sulfuric acid and 147 grams of nitric acid and combine them in a magnetically stirred 500 m
l flask suspended in an ice water bath. The ice water bath needs to have at least 2 inches clearance on all
sides from the flask and should have an inch or so clearance from the bottom of the flask."
Oh fuck! Chuck's mag stirrer isn't working very well anymore.
"Get the stirring going and keep a good vortex throughout the reaction. Put a thermometer in the flask and
note the temperature, it should be around 18C before you start. Now measure 100g of toluene into a beaker
and pour 5ml of it into the stirring acid solution. You'll see the toluene turn brown as it reacts, this brown
liquid will splash on the sides of the"
Now we know Chuck's stirrer isn't working the way it should. He understands the danger here
"Possible screwups: Don't screw this one up, recovery from it may require time in the hospital"
Can he use overhead stirring here? His only 500ml flask is single neck. If he uses the overhead
stirring he can not measure the temp, right? That's ok he can add the toluene slowly(1 ml rather than 5ml)
" Wait for the brown to turn yellow, this will take from a minute to several minutes"
Chuck will also wait longer after adding toluene. He will be careful, he understands the danger
"NEVER LET IT RISE ABOVE 60C"
Or. . . . Could Chuck use his 1 L 2 neck fb flask? Is there a rule of thumb when changing flask sizes
(using something other than reccomended in the synth)? Could using too large or small of a flask(within
reason)have negative results?
"The only way to get the newly created o-toluidine out of the flask is by steam distillation"
Chuck will set up using his pressure cooker for steam distill per Dwarfer.
" and use a 1 liter flask as the receiver. In the other hole of the flask put a bent glass rod that ends near the
bottom" & ". As the water boils it will force steam into the 1 liter distilling flask"
Oh fuck! Chuck doesn't have another 1 L flask. He wants to use his 500ml flask.
"The receiving flask will contain around 700 ml of yellow stained water and blobs of redish brown o-toluidine"
Well, fuck! Chuck's 500ml won't be big enough. Can he do this in 2 steps? 350 ml? Sure he can, right?
"In a suitable size flask (250 ml will do it here) put the o-toluidine with three times the volume of water and
about a teaspoon full of NaOH"
Chuck has a 250 Erlenmeyer flask and a 500ml RB. What was the rule of thumb about using different
sized flasks than the synth called for? Is it usually ok to go up or down 500ml?
" Use 1300ml of water and dissolve 20 grams of N-acetyl-o-toluidine and 50 grams of magnesium sulfate in it
with stirring while raising the temperature to 80C"
Chuck ain't got no 2+ L glass vessel. He will use the pressure cooker he used to steam distill this
should be ok, right?
CheapSkate seems to thinks so: " The entire mixture will work in a large Visions saucepan."
"Put 10 grams of N-acetyl anthranilic acid in a large test tube and add 10 grams of o-toluidine. There probably
isn't enough o-toluidine to get all the anthranilic wet" & ". As the o-toluidine heats up, it will dissolve the
anthranilic and condense on the side of the tube about half way up. The spreading o-toluidine will eventually
dissolve all the anthranilic and start to turn dark"
Chuck has a 100ml Erlenmeyer flask. Is this ok? Or does this 'reaction' require a tight space to climb,
dissolve and condense.
"Slowly raise the temperature to about 150C" & Continue raising the temperature over the next 30 minutes
until you reach 190C and keep it there" & "and suspend the test tube in a small visions sauce pan filled with
cooking oil over a hotplate"
What the fuck? How does Chuck take the temp of his test tube?
"Don't make the mistake of trying to mix or compress or in any way mess around with the chemicals in the test
tube"
That rules out the idea of sticking a therm in the test tube. Should he just take the temp of the oil bath?
What does chuck do about thermal lag? Won't the temp of the bath be warmer than the tube?
"Allow the solution to cool until just above room temperature and add 10ml 34% HCL"
Oh fuck Chuck don't have 34% HCL. The fucking search engine should help with this, right?
" Add 10% sulfuric acid a few milliliters at a time to the solution with stirring and the N-acetyl-anthranilic acid
will precipitate out."
Fuck! Chuck doesn't have 10% Sulfuric Acid. Same as above, right? UTFSE!"
". Now continue the boil until about 20% of the MeOH has been evaporated" & After about an hour there will
be crystals forming and clinging to the sides of the tube, wait until you're sure all the crystals have formed
and filter"
[red] Chuck doesn't have any tubes. However, he has a 100-1000ml Erlenmeyer flask. Could he one of
these instead
Lastly Chuck was curious. . . What is the yield? That cheapskate fellow forgot to say.
MaDMAx seems to gives us his yields here Post 246642 (MaDMAx: "Re: Quaaludes: Cheapskate scaled up", Methods Discourse), I think?
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(Chief Bee)
02-02-03 11:49
No 403672
Chuck should REALLY go get himself more equipment before attempting to synthesize anything.
What you suggest is like inviting a girl for dinner, where you both drink from the same wine bottle (because you don't have any glasses), while you eat on a saucer, and she on a paper plate. She can eat with your only fork and your bread knife because she's your guest, it doesn't matter to you if you have to eat with your hands. Dessert is no problem, as the ice cream comes in its own plastic container, after rinsing the fork and the knife in the sink, you can simply re-use them to cut/dig out the ice-cream together...
While the above technically works (just like your writeup), it doesn't look like a successful dinner, right?
Why do people think they can cut back 95% of their budget when doing chemistry, when they wouldn't dream of doing it when dating a girl? The result after the dinner/synthesis will probably be very similar - you won't be getting any!
(Stranger)
02-02-03 12:42
No 403702
Chuck is making some ludes, you comming over for dinner(yummie).
Why do people think they can cut back 95% of their budget when doing chemistry
People assume it's ok with chemistry because it works - per your page. Gotta use what ya got on hand. Although you may not fully support cutting it seems you obviously ar not 100% opposed:
* Build your own still g
* Do it yourself buchner funnel (PDF)
* Cheaply made Glove Box
* Improvised Overhead Stirrer
* Homemade microgram scale
* Construction of a Liebig condenser from copper tubing
Isn't there a synth on your page that reccomends using soup cans as some sort of vessel. Give Chuck alittle credit. He had all the necessary equipment. Now he almost has all the necessary equipment. . . Remember when Aqua girl and others used to rummage through the trash to find 'interesting' items to make push pull tanks with. Ya gotta use what you got.
While the above technically works (just like your writeup)
Thanks that's what I needed to know. My hero Chuck thanks you as well. I do have a question though. Is their a rule of thumb when picking a flask size?I remember someone saying when doing a distillation never fill the flask more than 3/4 full. Can this be plastered across the board? I understand 10ml of liquid in a 22L flask is overkill. However, not going to extremes and using alittle common sense can a flask ever be too large?
PS -
Chuck thanks you. Well, atleast I do. Now I can start and hopefully finish my story. If anyone cares to elaborate on the Chief's respons your comments are welcomed.
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(Chief Bee)
02-02-03 13:49
No 403721
I was not critizising the possibility of using improvised things, as long as you have adequate improvised labware handy. You really need to aquire a collection of more heat-resistant reaction vessels, which preferably would consist of pyrex round-bottomed flasks with ground-glass joints. If that is not available, go for next best, but there is always a limit to how much you can cut back on the equipment without your yields suffering so much as to become nonexistant.
For example, if you need to stir and take the temperature of the reaction mixture at the same time, you either need a magnetic stirrer or a three-neck flask, you cannot skimp on both things (as you cannot use an overhead stirrer and a thermometer in the same flask neck). A three-neck flask is cheaper than a magnetic stirrer, but if the former is absolutely unavailable to you, you can always construct your own mag-stirrer with a little elbow grease (instructions at my page).
Some tips: A3/4 full flask is to push it somewhat, if possible then always work with flasks 1/3 to 2/3 full. Even less than that if you intend to perform a reaction which may boil violently, foam, bump or otherwise might bounce out of the flask if it is too small.
If your glassware is too small to contain the amounts of chemicals suggested in a writeup, then scale down (divide all the weights and volumes in half, but keep reaction times and temperatures the same), and if need be, run the reaction twice to accumulate the necessary amount of precursor for the next step.
A flask cannot really be too large (within reasonable limits) when doing a reaction, but it can definitely be if you are distilling, as the product will just condense on the walls of the flask instead of distilling over. You need to fill a flask to at least 1/5 when distilling, or else you will lose too much.
(Stranger)
02-05-03 22:37
No 404967
I quickly put this together to assist me in writing about Chuck. It has been paraphrased and shortened. All credit is due to CheapSkate. I also find this an easier format to reference if I have any questions.
Caution written by a non-chemist. Has not yet been checked for errors
The chemicals you have to buy:
* Sulfuric Acid - 294g (additional will be needed * )
* Nitric Acid - 147g
* Toluene - 100g
* Distilled water - Gallon or two
* Iron filings - 120g
* Hydrochloric Acid - 20ml
* Sodium Hydroxide - 3 teaspoons *
* Glacial acetic acid - 100ml
* Acetic Anhydride (optional, see below) - 50ml
* Potassium Permanganate - 50g
* Acetone - approx 1 L
* Methanol - approx 1 L
* Denatured Alcohol -approx 1L
* Mag Sulfate - 50g
*Amounts are unknown. However, not much is needed.
Equipment:
* Boiling granules
* 1 L 2 Neck flask
* Separatory Funnel (1 L or larger)
* Thermometer
* Hotplate / Stirrer or overhead
* 200mm Condensor(400 reccomended by Cheapskate)
* Test Tube
* Thermometer adapter
* 2 + L flash or other large vessel(Cheapskate uses visionware)
* Latex Gloves
* Steam (Use a pressure cooker. Cheapskate uses a 2L elnmr flask)
* Tubing(Glass reccomended by Cheapskate)
* 250ml glask
The details:
Making nitrotoluene:
This is dangerous. If the reaction gets out of control, there is a good possibility of explosion. So follow instructions and keep the temperature down.
1) Take 294 grams of sulfuric acid and 147 grams of nitric acid and combine them in a magnetically stirred 500 ml flask suspended in an ice water bath. Have 2 inches of clearence on all sides of(Make sure flask can move). Temperature of flask should be 18c or lower before proceeding.
2) Now measure 100g of toluene into a beaker and pour 5ml of it into the stirring acid solution. The toluene will turn brown as it reacts. Wait for the brown to turn yellow, this will take from a minute to several minutes depending on how much toluene you actually added. Now add another 5 ml
toluene and wait for it to turn yellow. Continue this until you have added all the toluene. Allow tempature to drop to 20c between toluene additions and never let the temp rise above 60c. If it does you may die.
3) After the addition of all the toluene, let the solution set with continued stirring for 4-5 hours.
4) Grab sep funnel. Seperate the nitrotoluene from the acid layer(Nitro will be a much lighter yellow).
5) Clean the 500ml flask. Add 2x the volume of the nirto of water and a teaspoon of NaOH. Stir until NaOH dissolves. Water layer will be orange and the nitro will have turned a bright yellow. Keep nitro layer.
6) Seperate both layers. Rinse 500 ml flask, again. Follow step 5 but no NaOH this time. Repeat step 5 without NaOH until water layer does not turn orang). Eventually water will just have a yellow tint.
Yield approx 150ml of bright yellow nitrotoluene.
Making o-toluidine:
1) In a 1 liter 2 neck distillation flask fit an overhead stirring device in the center hole. Pour 60cc of water,
120 grams of powered iron and the 150 ml of nitrotoluene into the flask and start stirring. The stirring must be vigorous.
2) While stirring add 10 ml of the HCl to the flask and wait for about 15 minutes. When flask is cool enough to handle continue.
3) Add 5ml of Hcl, wait for flask to cool(30 min) then add another 5ml of hcl.
4) Allow things to cool and settle for a couple of hours.
5) Set up for steam distillation. Fit distillation adapter to center hole and use 1L flask for receiver. In other hole you will need to deliver steam. Cheapskate suggests using a bent glass rod connected to the flask by a thermometer adapter. Then connect the rod to a 2L Erlenmeyer flask(This will be source of steam)
6) Seperate water from o-toluidine.
7) Place o-toluidine with 3x volume of water and a teaspoon of NaOH in a 250ml flask
8) Boil 'briefly' and stir. Remove from heat & watch. O-toluidine should 'surface'.
9) Pour solution through filter to remove solids.
Yield approx 30ml of O-toluidine
Making N-acetyl-ortho-toluidine:
Using Acetic Anhydride:
step skipped(See cheapskate writeup)
1) Attach 400mm condenser to a 500ml round bottomed flask. Put in 50ml of o-toluidine and add 100ml of
glacial acetic acid through the condenser. The fluids only condense up about 2cm into the condenser. Reflux for 3 hours. **
2) Dump the contents directly into a 1 liter flask filled to 900ml with room temperature dH2O. Pink crystals will immediately form.
3) Cool the solution in the freezer until cold, but don't freeze.
4) Filter the crystals with suction and save the mother liquid.
5) Using gentle heat from a lamp dry the crystals and recrystalize by using just enough boiling hot alcohol
to dissolve them. Now cool the alcohol in a freezer for 15-20 minutes.
6) Vacuum filter the recrystalized product from the solution and save the solution in the same flask as the first filtration thereby saving all the liquid.
7) After about an hour the mother liquid will have formed crystals also. Filter this and combine with the first product, wait a couple of hours to make sure it has all crystalized.
**Solidifaction process skipped. See Cheapskate Write Up for details
Yield was 43 grams of white needle like crystals.
Making N-acetyl-anthranilic acid
1) In a 2 L + vessle add 1300ml of water and dissolve 20 grams of N-acetyl-o-toluidine and
50 grams of magnesium sulfate in it while stirring
2) Slowly raise temp to 80c to dissolve the N-acetyl-o-toluidine. This will take a few minutes. At 80c crystals should dissappear.
3) Add 50 grams of potassium permanganate, increase the stirring speed to keep the solution from settling.
4) Stir solution for 3 hours at 85-90c. Add water as necessary.
5) Neutralize solution with 30ml of denatured alchol. Solution should turn brown and pink fluid should
disappear. Add another 10ml of denatured alchol if solution is still pink.
6) Filter solution hot, with suction. Be sure to get as much of the solution as possible
7) While stirring ad 10% sulfuric acid a few ml at a time. The N-acetyl-anthranilic acid will precipitate out.
8) Filter and clean by dissolving in weak NaOH and reprecipitate by adding sulfuric as before.
Yield 16 grams N-acetyl-anthranilic acid
Making Methaqualone
Method 1.
1)Put 10 grams of N-acetyl anthranilic acid in a large test tube and add 10 grams of o-toluidine. There probably isn't enough o-toluidine to get all the anthranilic wet, so add 4 ml more.
2) Suspend the test tube in a small visions sauce pan filled with cooking oil over a hotplate. Slowly raise the temperature to about 150C. Don't mess with what is in the test tube!
3) Allow heating o-toluidine to dissolve all the anthranilic, turning it black. If some anthranilic remains undisolved tilt and swirl the test tube.
4) Over the next 30 min raise the temp of the test tube to 190c. Water will be evolved from the reaction creating bubbles. Hold temp for 3 hours. **
5) Add 2x the volume of acetone. Stir until purple stuff dissolves.
6) Allow acetone to cool or HCL will boil. Add same volume of 34% hcl as purple stuff.
7) Bring entier solution to boil for 4 minutes, remove hear and allow to cool.
8) Allow solution to cool for 1.5 hours, crystals will form in the purple stuff. If necessary refrigerate solution.
If no crystals form, heat a glob of purple stuff return it to the flask and stir.
9) Filter the crystals dry and proceed to purification!
Purification:
1) Dissolve crystals in beaker by boiling with 2x amount of Acetone & boiling stones.
2) Filter the crystals and dry.
~If, after drying, there is a purple tint to the crystals, then recrystalize from
methanol. Put crystals in a small beaker add enough MeOH to get them wet and start
heating the mix. If crystals don't dissolve bring the MeOH to a boil and add MeOH a little more,
boil until they have all dissolved. Boil until about 20% of the MeOH has been evaporated. Allow the
solution to cool and wait. Crystals will form in about an hour, wait until you're
sure all the crystals have formed and filter. Use acetone to wash the crystals out of your flask and to rinse
as much of the nasty-purple-stuff from the crystals in your filter paper. Save the solution and the crystals. ~
3) Now repeat the acetone boil described above and filter and dry. You should have light steel grey to white
powder, if you do, stop and put this batch aside, if you don't, wash with acdtone again.
4) Take purple solution you saved from recrystalization, add boiling granules and boil away half the volume.
5) Allow this to cool and methaqualone will precipitate. Purify with acetone as above(if necessary) and add to
your completed batch. You can repeat this process until almost all the methaqualone has been recovered from the solution, but each recovery will be less pure. If you choose to do this, combine all the recovered product and do one last acetone boil to clean it up.
Method 2.
(Skipped see Cheapskate Write Up)
Method 3:
(Skipped see Cheapskape Write Up)
Super purification:
1) Mix up two flasks of water at ph 3 and add your methaqualone.HCl to one of them. Boil the methaqualone
until it dissolves in the acidic water, some stuff will not dissolve.
2) Filter the boiling hot solution into a suitable flask and rinse the filter paper through the funnel with the
other flask of hot water. Allow the water to cool and chill to recover the crystalline methaqualone.HCl.
**This will be pure white fluffy crystals with the only contaminant left being the filter fibers that you scrap off
when you gather the crop! WOOHOO! **
Yield ??? ??? of (white??) methaqualone crystals
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