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gsd
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As usual excellent work Magpie!
Only suggestion I would like to make it is to keep your SnCl4 in a bottle with PTFE lined closure as SnCl4 has got a nasty habit of freezing the glass
to glass joint.
Also it is extremely hygroscopic liquid. Preferably it should be stored in a double bottle (Bottle in bottle), or utilized immediately.
gsd
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Magpie
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Thanks gsd! I did place it in a narrow neck 100mL Qorpak bottle with ptfe lined lid. Perhaps I should also dip the head in paraffin wax. This seems
to be working well to contain my PCl5.
The single most important condition for a successful synthesis is good mixing - Nicodem
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gsd
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Have you planned any specific reaction with SnCl4?
With this versatile reagent in hand it opens up whole new field of Organotin compounds for you.
You have already made n-Butyl Bromide and its Grignard. With SnCl4 you can now make Butyl tin chlorides and Tetrabutyl Tin.
gsd
[Edited on 14-4-2016 by gsd]
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Texium
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Magpie, excellent write-up as always, but I just thought I'd point out that the procedure that I used several posts upthread of yours was essentially
the same albeit with a less sophisticated apparatus and on a much smaller scale. Though your attempt was clearly more successful and more
well-written-up, I feel I still deserve some recognition for being the first to document the procedure on the forum.
All that aside, I hope to try it again sometime in the next couple months, after I finish installing the exhaust fan in my new lab space. On my first
attempt the fumes were so bad it kept me from wanting to even open the vial again, much less make more.
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Magpie
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gsd that is good to hear that this new reagent will be so useful. I had a much more modest use in mind: making thymolphthalein.
zts16: I didn't mean to slight your accomplishment. It was, in fact, encouragement to me that Brauer's procedure would actually work.  I'll add a note to my post in edit.
The single most important condition for a successful synthesis is good mixing - Nicodem
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DJF90
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@Magpie - It looks as if your product may be suffering from contamination with dissolved chlorine. Perhaps a reflux period prior to distillation or
sparging with dry air/nitrogen/argon will yield a colourless product.
Quote: Originally posted by zts16  | Though your attempt was clearly more successful and more well-written-up, I feel I still deserve some recognition for being the first to document the
procedure on the forum.
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Pretty sure this was documented several years ago on Versuchschemie...
[Edited on 14-4-2016 by DJF90]
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blogfast25
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Very nice work, Magpie.
It would be nice to try the product as an FC alkylation catalyst.
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Magpie
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| Quote: Originally posted by DJF90 | @Magpie - It looks as if your product may be suffering from contamination with dissolved chlorine. Perhaps a reflux period prior to distillation or
sparging with dry air/nitrogen/argon will yield a colourless product.
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Thanks for the suggestion! If I think that the Cl2 will be a problem with an intended synthesis I will reflux/purge it out.
This is a real shame to see the demise of a fine amateur chemistry forum, especially if due to internal squabbles. I learned a lot from
versuchschemie.de.
Thanks. Yes, that is my intention. Thymolphthalein is made using an FC alkylation using phthalic anhydride, thymol, and SnCl4. I had a hard time
finding a procedure for this.
The single most important condition for a successful synthesis is good mixing - Nicodem
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aga
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Superb work Magpie !
Excellent to see some practical chemistry in action.
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Magpie
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Belated thank you aga.
Here's a picture of my SnCl4 storage bottle. The cap has a ptfe liner. It looks like I am going to have to dip the cap/neck in paraffin.
The single most important condition for a successful synthesis is good mixing - Nicodem
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blogfast25
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| Quote: Originally posted by Magpie | Belated thank you aga.
Here's a picture of my SnCl4 storage bottle. The cap has a ptfe liner. It looks like I am going to have to dip the cap/neck in paraffin.
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Also: don't drop that bottle. It's damn heavy, that stuff!
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Magpie
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Maybe I should leave it "as is," assuming the white, solid tin material is forming a seal?
The single most important condition for a successful synthesis is good mixing - Nicodem
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blogfast25
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If it's SnO2 forming you may have trouble opening the bottle at some point. I'd at least tape it up.
[Edited on 20-5-2016 by blogfast25]
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Rhodanide
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Tin (IV) Chloride synthesis & apparatus questions
Hi folks,
Since dehydration of Sn(IV) Chloride * 5 H2O seems to be out of the question, I think that I should just go for the anhydrous. How should I
set up the apparatus? What kind of apparatus would I need? My plan is to use a 2-neck, 500mL or 1L RBF with around 100-150 g or so of mossy Sn, with
the first neck being the Chlorine inlet (still figuring out how to do this), and the second (top) neck being the takeoff for the (hopefully) anhydrous
SnCl4. Now, should I use a normal condenser? I'm hesitant to do this because I don't want the cold water to condense any water from the
atmosphere, therefore decomposing any Tetrachloride which may be distilling. My plan for actually RUNNING the synthesis is melting the tin with a
propane torch on low setting, so as to avoid needless thermal shock on the RBF. Then, in a separate 250 mL 2-neck RBF, I'll add some powdered TCCA.
I'll attach a takeoff adapter to the canted neck, and an addition funnel loaded with HCl on the vertical neck. Chlorine will be generated, and led
into the molten Sn. I don't plan on bothering to make a drying "thingy" because I can't afford a gas wash bottle. Once the Cl is led into the molten
Sn, the SnCl4 should distill out due to the temperature and condense. The 'tet should be obvious due to the smoke. How would you all tweak
this synth? Does it sound like it would work?
Thanks,
-R
[Edited on 4-25-2018 by Rhodanide]
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CharlieA
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Out of curiosity, can you please share any literature references for this procedure?
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yobbo II
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https://geocitieschloratesite.000webhostapp.com/chlorate/mak...
http://www.sciencemadness.org/talk/viewthread.php?tid=1218
http://www.sciencemadness.org/talk/viewthread.php?tid=12826&...
http://www.sciencemadness.org/talk/viewthread.php?tid=29645
https://www.sciencemadness.org/whisper/files.php?pid=118256&...
Some info.
[Edited on 26-4-2018 by yobbo II]
Edit by Texium: removed now-redundant link
[Edited on 4-26-2018 by Texium (zts16)]
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Sigmatropic
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I wouldn't omit the drying part. A tube with CaCl2 or better yet a wash bottle with sulfuric acid isn't all that complicated.
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Geocachmaster
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Yes, you should dry the Cl2. If you don't have a drying tube or Drechsel Bottle, just use a two hole stopper and an Erlenmeyer flask. To
get chlorine in the flask, use a thermometer adapter like this and some glass tubing. You could also use very long glass tube and run it in from the top of the still head if you are missing the
glassware. For your condenser, just use room temperature water. SnCl4 boils at over 100 C so this should be fine. No condensation will form
with room temp water.
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Rhodanide
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| Quote: Originally posted by Geocachmaster | | Yes, you should dry the Cl2. If you don't have a drying tube or Drechsel Bottle, just use a two hole stopper and an Erlenmeyer flask. To
get chlorine in the flask, use a thermometer adapter like this and some glass tubing. You could also use very long glass tube and run it in from the top of the still head if you are missing the
glassware. For your condenser, just use room temperature water. SnCl4 boils at over 100 C so this should be fine. No condensation will form
with room temp water. |
Perfect. Thanks, T!
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Rhodanide
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PERFECT. THANKS!
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DJF90
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You don't need to heat the tin to get it to react. See Brauer in the forum library, p729, for a detailed preparation.
This should have been one of the first references you consult before even starting a thread asking about it.
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Rhodanide
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| Quote: Originally posted by DJF90 | You don't need to heat the tin to get it to react. See Brauer in the forum library, p729, for a detailed preparation.
This should have been one of the first references you consult before even starting a thread asking about it. |
Sorry, I'm not experienced with looking for things like that, in fact I didn't even know I could do that. Um, where exactly would I find that?
Edit: Found it after a Google search
[Edited on 4-26-2018 by Rhodanide]
[Edited on 4-26-2018 by Rhodanide]
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Texium
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Threads Merged
26-4-2018 at 09:35 |
Magpie
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Did you read this thread?
References
1.Handbook of Preparative Inorganic Chemistry, 2nd ed, by Georg Brauer (1963), forum library.
2. “Chlorine – Illustrated Practical Guide,” by Len1, Prepublication http://www.sciencemadness.org/talk/viewthread.php?tid=9713
3. “Building a Peristaltic Pump for Small Volumes/Rates,” post by Magpie, http://www.sciencemadness.org/talk/viewthread.php?tid=59870#...
Questions, suggestions, and comments are welcomed.
The single most important condition for a successful synthesis is good mixing - Nicodem
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CharlieA
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