Author Topic: Short Question Thread 2.0  (Read 5707 times)

Happyman

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Re: Short Question Thread 2.0
« Reply #160 on: August 30, 2012, 12:28:41 AM »
Quote
It's probably coming out the exhaust   ;)  Oil pumps aren't generally used for distilling ether since it's so volatile 8)

Already figured that one out the hard way  :D. I have the exhuast running outside.
« Last Edit: August 30, 2012, 12:30:23 AM by Happyman »

Happyman

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Re: Short Question Thread 2.0
« Reply #161 on: August 30, 2012, 02:59:58 AM »
I figured it out. I'm just a noob as usual. The valves that control the vacuum just pull in outside air, causing ether to leak.

Tsathoggua

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Re: Short Question Thread 2.0
« Reply #162 on: August 30, 2012, 06:42:50 AM »
Can K2CO3 serve as the base when acylating a phenol using the acyl halide?

Substrate in  mind is oxycodone, to form the propionyl ester.
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I'm hyperbolic, hypergolic, viral, chiral. So motherfucking twisted my laevo is on the right side.

atara

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Re: Short Question Thread 2.0
« Reply #163 on: August 31, 2012, 01:27:15 AM »
I believe it should work fine, yes, but oxycodone is not a phenol. I assume you mean oxymorphone. If not, consider this review: Recent advances in ether dealkylation.

Since K2CO3 releases water on protonation, using an excess of acyl halide may increase yield. I have also seen pyridine used: http://www.orgsyn.org/orgsyn/prep.asp?rxntypeid=117&prep=CV9P0507
« Last Edit: August 31, 2012, 01:47:10 AM by atara »

Tsathoggua

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Re: Short Question Thread 2.0
« Reply #164 on: September 02, 2012, 02:52:32 AM »
Aniline would be an easier org. base to prepare here. Or possibly piperidine.

Toady was thinking of esters at the -14 position hydroxyl actually.

Atara, do you have the full txt of that available?
« Last Edit: September 02, 2012, 04:47:06 PM by Tsathoggua »
Nomen mihi Legio est, quia multi sumus

I'm hyperbolic, hypergolic, viral, chiral. So motherfucking twisted my laevo is on the right side.

Assyl Fartrate

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Re: Short Question Thread 2.0
« Reply #165 on: September 02, 2012, 04:31:51 AM »
Aniline and piperidine will be acylated. You need a tertiary amine, if that is the road you choose to travel.

If your goal is to acylate the 6-keto moiety, yielding an enol ester, you should use pyridine if possible, though it's possible carbonate could work with some sacrifice in yield. Better may be to use propionate salts to generate propionic anhydride in situ and also to act as a base.

Quote
Kelentei, I. B.; Stenszky, E.; Czollner, F.; Meszaros, Z.; Szlavik, L.
"Preparation and pharmacological action of morphine derivatives."
Pharmazie 1957, 12, pp.600-7

Abstract

14-Acetoxydihydrocodeinone enol acetate (I) and 3-acetyldihydromorphinone enol acetate (II) were prepared and biotested.

Dried dihydrohydroxycodeinone in Ac2O was refluxed with AcONa at 160-70°C for 2 1/2 hours, cooled, the excess Ac2O removed, the acetylated base precipitated with diluted ammonia with agitation at under 15°C, kept standing, filtered, and recrystallized, giving 88-90% I, mp. 209-10°C (from EtOH); 1 part was soluble in 30 parts of EtOH, 2 of CHCl3, 4 of C6H6, 100 of ligroine, 100 of Et2O, and 50 of Me2CO (at 20°C).
« Last Edit: September 02, 2012, 05:52:17 AM by Assyl Fartrate »
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2bWinston

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Re: Short Question Thread 2.0
« Reply #166 on: September 02, 2012, 05:38:16 PM »
Hi, I want to do a qualatative test on what I think is 2-bromo-1-phenylpropane. I have thought that if I disolve some silver nitrate in water, and add that to the sample, it would precipitate insoluble silver bromide. I havent, done this before, and just helping out a friends friend who happened to come accross a solution, yellow red, that he was led to believe was the above mentioined molecule. I do not have experience with bromosafrole nor with saffrole so any hints would be good. Thanks in advance.

ps, I had to change my name because I couldn't recall the password, and cant get into hotmail.


2bWinston

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Re: Short Question Thread 2.0
« Reply #167 on: September 03, 2012, 10:09:15 PM »
update, dissolved some silver nitrate in ethanol, took time, then added that to small amount of sample, blackish color ppt. I initially thought of disolving the silver nitrate into water, but if a silver halide gets formed, it to would disolve in the water, so changed to dry as poss (non sodium methods) ethanol. Took abit to disolve, but finally did and the black ppt took 20 odd minutes.????

Oerlikon

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Re: Short Question Thread 2.0
« Reply #168 on: September 04, 2012, 12:46:21 AM »
Hy,

Can anybody suggest me any kind of easy to get,bitter as hell,water soluble thing.
It's family mather.
I need something bitter to put into methadone bottle so  they think it's methadone which is unholy bitter.
Medicine,chemical,anything...

Used to filter OTC codeine meds to get codeine in the water but it isn't bitter enough.
Any suggestion are welcome.
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Assyl Fartrate

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Re: Short Question Thread 2.0
« Reply #169 on: September 04, 2012, 12:51:56 AM »
That would be denatonium. 10ppm is intolerably bitter to most.

Xanax, Ambien, and Benadryl are all very bitter, but there's different qualities in the taste.
« Last Edit: September 04, 2012, 08:33:34 AM by Assyl Fartrate »
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Oerlikon

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Re: Short Question Thread 2.0
« Reply #170 on: September 04, 2012, 05:15:18 PM »
Yeah but xanax is pitty to waste,Ambien I don't have and Benadryl has very distinct "aroma".
Also tried with quinine but you cant buy it here just like that (OTC)
After tasting my medical cabinet found ranitidine to suit my needs but solution is tan.

Thanks anyway!
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4studiesonly

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Re: Short Question Thread 2.0
« Reply #171 on: September 04, 2012, 08:10:14 PM »
Why mess about with stuff that has a good purpose like xanax,ambien etc...

As assyl fartrate stated denatnium will do the job like nothing else. In my country its used in anything that you can get drunk/intoxicated with, as ethanol or methanol or any kind of alcohol which are not meant for consuming and sold/taxed by the state (IPA excluded). I think, almost sure, its also used in such a thing as the colourless nail polish you put on kids nails when you want them to learn not to bite them.
Bis zum bitteren ende

Happyman

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Re: Short Question Thread 2.0
« Reply #172 on: September 06, 2012, 10:36:37 PM »
Hey guys, I have another vacuum related question, what type of oil goes in to an oil (vacuum) pump fron a lab. I was thinking of using compressor oil.

lugh

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Re: Short Question Thread 2.0
« Reply #173 on: September 07, 2012, 12:07:21 AM »
Quote
Hey guys, I have another vacuum related question, what type of oil goes in to an oil (vacuum) pump fron a lab. I was thinking of using compressor oil.

Refrigeration compressor oil will work quite well, but you really need to start doing your own research:

h**p://www.belljar.net/index.htm

h**p://www.repairfaq.org/sam/lasercva.htm#cvaoilc

h**p://www.tau.ac.il/~phchlab/experiments_new/SemB02_Vacuum/01Home.html

instead of expecting some one else to do it for you   ::)  The end results from the effort applied   8)
Chemistry is our Covalent Bond

Electro´S

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Re: Short Question Thread 2.0
« Reply #174 on: September 07, 2012, 03:16:09 AM »
All right!
« Last Edit: September 07, 2012, 08:50:39 AM by Electro´S »

lugh

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Re: Short Question Thread 2.0
« Reply #175 on: September 07, 2012, 06:44:14 AM »
Quote
What you choose???

And for Al/Hg, What is the rate of Al/Nitro compound without the famous double bound?? It would be run just in IPA or Methanol instead of AcOH/IPA  like nitroalkenes?

As you were told already in:

http://127.0.0.1/talk/index.php/topic,2962.msg32960.html#msg32960

you are making a nuisance of yourself  ::)  As mentioned in:

https://the-collective.ws/forum/index.php?topic=9679.0

spoonfeeding is contrary to your personal development in learning chemistry  ;)  Clandestine Chemistry is simply too dangerous for short cuts  :(  As far as the Christmas reduction:

http://www.erowid.org/archive/rhodium/chemistry/nitrostyrene.reduction.alhg.html

should have been memorized by now  :o  An old Hive thread about the subject in question has been posted:

https://the-collective.ws/forum/index.php?topic=23176.0

so there had better not be any more questions about this particular subject in this thread  :-X  There's no way anyone can choose what's best for you since circumstances can differ greatly  :P The end results from the effort applied  8)
Chemistry is our Covalent Bond

Happyman

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Re: Short Question Thread 2.0
« Reply #176 on: September 07, 2012, 05:09:34 PM »
Quote
Hey guys, I have another vacuum related question, what type of oil goes in to an oil (vacuum) pump fron a lab. I was thinking of using compressor oil.

Refrigeration compressor oil will work quite well, but you really need to start doing your own research:

h**p://www.belljar.net/index.htm

h**p://www.repairfaq.org/sam/lasercva.htm#cvaoilc

h**p://www.tau.ac.il/~phchlab/experiments_new/SemB02_Vacuum/01Home.html

instead of expecting some one else to do it for you   ::)  The end results from the effort applied   8)



Thanks you very much, I yield to superior research skill.
But seriously how did you find that? Neither Myself nor the hardware employee that helped me ??? for an hour could find anything. The closest I can was some guy at the collective saying it was mineral oil  ???
« Last Edit: September 07, 2012, 05:13:43 PM by Happyman »

carl_nnabis

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Re: Short Question Thread 2.0
« Reply #177 on: September 07, 2012, 11:09:07 PM »
I have a question about grignard suited solvents: I want to use DIPE, diisopropyl ether, to substitute diethylether with because it sucks to get the latter as i have to pick it up in person from holland if i want to get more than a quart liter, and without getting pretty much embezzled from the local pharmacys.
I dont think the schlenk equilibrium will lead to a different favored alkylmagnesiumbromide in both solvents, that means they are interchangable there, am I right on this one? Both are monoethers, and Ive seen only triethylamine and dioxane so far giving another formula of alkylmagnesium halide, and both are substantially very different to a monoether like Et2O or DIPE, so thats where i need affirmation please.
I would also likely use another well suited solvent, like THF of course. Has anyone first hand experiences with grignards using other solvents as Et2O? Pyramid, you were meant, chime in and tell! ;D

And I do have another question, how do I keep DCM from giving a small second layer on top of the solution thats getting extracted? It really bothers me all the time it is doing this and salting out doesnt work, in acidic solutions too.
Cooling it very muich also doesnt help.
Maybe adding a bit of a solvent miscible with DCM but less dense than water will collect the tiny upper DCM layer, and will dissolve it in the main portion DCM on the ground?
Also i got a bit carbon monoxide poisoned once I worked with DCM, everybee working with it and does stuff like redistilling large amounts of it without a fume hood should bee aware it gets metabolized into CO which is toxic like HCN, when accidentally inhaled.
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lugh

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Re: Short Question Thread 2.0
« Reply #178 on: September 07, 2012, 11:55:22 PM »
Quote
I have a question about grignard suited solvents: I want to use DIPE, diisopropyl ether, to substitute diethylether with because it sucks to get the latter as i have to pick it up in person from holland if i want to get more than a quart liter, and without getting pretty much embezzled from the local pharmacys.

Please read both:

https://the-collective.ws/forum/index.php?topic=10580

and

https://the-collective.ws/forum/index.php?topic=12796

for more information  ;)  The middle layer is an emulsion, the elimination of which takes a long time under the best circumstance  ::)  DCM is notorious for forming stable emulsions which complicate matters greatly  8)

Chemistry is our Covalent Bond

Oerlikon

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Re: Short Question Thread 2.0
« Reply #179 on: September 08, 2012, 02:16:35 AM »
Does anyone have idea how to separate DAM aka. heroin from caffeine!?

I stumbled upon source of great quality 50/50 DAM/Caffeine and was promissed to get a free sample if I help
to separate it and get 100% pure DAM.

Now i know that DAM is in freebase form but I am not sure about caffeine.
I know that DAM freebase is not very soluble in water while caffeine is,so this might do a trick.
Shake it in the warm water,caffeine should dissolve leaving DAM to be filtered.

Does anyone have an idea if this will work or what other solvent to use?!

Vice versa or dissolving DAM while leaving caffeine is good idea too if someone knows how to do it.
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