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IndoleAmine
Dreamreader Deluxe
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| Joined: 09 Feb 2005 |
| Posts: 681 |
| Location: Bahamas |
18717.10 Points
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Sun Feb 20, 2005 3:17 pm |
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Who left out anything? 
the whole thing is very simple: add enough lye to cassia oil to maintain a pH between 12-13, reflux for some hours - and steam distill the heck out of it. Rocket science, so to speak. 
Result: acetaldehyde and benzaldehyde, easily separable via vac distillation...
(the surfactants and stuff are only for more ease when working with such huge amounts, I would guess)
i_a |
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java
Consumer
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| Joined: 07 Feb 2005 |
| Posts: 736 |
| Location: The Mexican Republic |
21794.14 Points
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tina_craig
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| Joined: 07 Feb 2005 |
| Posts: 26 |
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642.42 Points
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Fri Mar 11, 2005 3:25 am |
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| So, its really that easy? Cassia oil, lye solution and distill. Hmm, cool. |
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IndoleAmine
Dreamreader Deluxe
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| Joined: 09 Feb 2005 |
| Posts: 681 |
| Location: Bahamas |
18717.10 Points
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no
Fri Mar 11, 2005 10:19 am |
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No, not lye solution. Solid NaOH/KOH, as much as to keep pH between 11-13, and reflux for 1h.
THEN add water and steam distill....
i_a |
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tina_craig
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| Joined: 07 Feb 2005 |
| Posts: 26 |
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642.42 Points
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Fri Mar 11, 2005 10:43 pm |
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| How much benzaldehyde could one expect back from 4 oz. of cassia oil? |
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n00dle
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| Joined: 03 Apr 2005 |
| Posts: 21 |
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745.88 Points
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Wed Apr 13, 2005 5:04 pm |
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| Anyone got refs using sodium perborate? |
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java
Consumer
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| Joined: 07 Feb 2005 |
| Posts: 736 |
| Location: The Mexican Republic |
21794.14 Points
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Phenylalanine to benzaldehyde
Wed Apr 13, 2005 7:18 pm |
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Here is a recent contribution by WizardX over at WD on the synthesis of benzaldehyde from phenylalanine...........java
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http://www.ajinomoto.co.jp/amino/e_aminoscience/bc/amino_13.html
Comment
Phenylalanine when heated in 5N sodium hydroxide at 110~115? for 5 hours, it decomposes forming benzaldehyde. |
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IndoleAmine
Dreamreader Deluxe
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| Joined: 09 Feb 2005 |
| Posts: 681 |
| Location: Bahamas |
18717.10 Points
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Wed Apr 13, 2005 8:36 pm |
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N00dle: the refs for all mentioned procedures are included in this thread, percarbonate is not amongst them.
Maybe it would work too, instead of persulfate? But I'm not sure..
The original persulfate oxidation patent (toluene/benzyl alcohol to benzaldehyde) can be read here (check example 5/page 4)...
greets
i_a
Last edited by IndoleAmine on Thu Apr 14, 2005 7:03 am; edited 1 time in total |
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anime
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| Joined: 13 Apr 2005 |
| Posts: 131 |
| Location: Planet Earth |
3517.62 Points
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Wed Apr 13, 2005 11:33 pm |
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Does anyone have references on converting benzyl chlorides to alcohols. (I know simple hydrolysis in a basic solution should yield the benzyl alcohol, but I am curious about the yields *%) obtained via this method).
I'm interesting in the synthesis of other substituted benzaldehydes.
How does this sound.
p-methoxytoluene is dibrominated.
persulfate oxidation to the aldehyde.
nucleophillic substition of the 3,5 bromine with NaOCH3 yielding a 3,4,5-trimethoxybenzaldehyde.
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IndoleAmine
Dreamreader Deluxe
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| Joined: 09 Feb 2005 |
| Posts: 681 |
| Location: Bahamas |
18717.10 Points
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Thu Apr 14, 2005 4:13 am |
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| Quote: |
How does this sound.
p-methoxytoluene is dibrominated
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Sounds like the Br's would not only go to their desired positions in this case, if you ask me.  |
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Sodium Persulfate
Thu Apr 14, 2005 6:46 am |
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In regards to a few posts back,
Indole mentioned a cheap and easy Persulfate Synth.
I agree that if a nice and OTC one can be made, then this is great route, considering the availability of Toluene as opposed to Cassia, or Apricot Kernl Oil.
Synth of Na2 S2 O8 , I'll have a look
syn |
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n00dle
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| Joined: 03 Apr 2005 |
| Posts: 21 |
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745.88 Points
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Thu Apr 14, 2005 2:20 pm |
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Completely stupid question but is there any way we can use peroxymonosulphate?
It's probably the stupidest thing ever written here but it seems to be a fairly gentle oxidiser. |
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BzCHO
Thu Apr 14, 2005 3:00 pm |
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oxone?
I have heard rumours, but have never seen a doocument |
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Esplosivo
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| Joined: 12 Feb 2005 |
| Posts: 9 |
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182.38 Points
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Re: Sodium Persulfate
Thu Apr 14, 2005 3:17 pm |
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| synthetika wrote: |
In regards to a few posts back,
Indole mentioned a cheap and easy Persulfate Synth.
I agree that if a nice and OTC one can be made, then this is great route, considering the availability of Toluene as opposed to Cassia, or Apricot Kernl Oil.
Synth of Na2 S2 O8 , I'll have a look
syn
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I'm not sure but doesn't electrolysis of a sulfate result in the production of its persulfate? IIRC I have heard about the conversion of ammonium sulfate to the persulfate for the oxidation of toluene to benzaldehyde. Hope this helps. |
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Esplosivo
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| Joined: 12 Feb 2005 |
| Posts: 9 |
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182.38 Points
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Thu Apr 14, 2005 3:30 pm |
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Her it is, the synthesis of potassium persulfate by electrolysis of potassium hydrogensulfate (bisulfate):
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Potassium persulphate, K2S2O8, must be regarded as a derivative of the liquid oxide S2O7, which was first obtained by Berthollet. The salt is obtained on electrolyzing a solution of acid potassium sulphate; it is sparingly soluble in cold water; in presence of water it is slowly decomposed yielding potassium hydrogen sulphate and oxygen. …
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If I find something about ammonium persulfate I'll post back soon.
Edit 1: OK found reference for the synth. of ammonium persulfate. It is done in the same way of potassium persulfate, simply by substituting potassium hydrogensulfate with ammonium hydrogensulfate. |
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