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Author: Subject: Everyday Chemistry (provisional)
DraconicAcid
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[*] posted on 21-3-2021 at 21:30


I spent a couple of hours typing up a document explaining substituents in organic chemistry, including the isoalkyls, neoalkyls, and various aromatic substituents. Saved it as a pdf and the computer ignored everything in the structures other than the R labels.

So every substituent is an R surrounded by white space.




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[*] posted on 22-3-2021 at 08:15


Anybody have any thoughts on acesulfame potassium (artificial sweetener) as a source for acetoacetic acid? Looking at the structure, I'm hopeful both the enol ester and amide can be hydrolyzed in one step by boiling with NaOH.



Reflux condenser?? I barely know her!
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[*] posted on 11-4-2021 at 09:53


INitroethane. Just a few ml, but I count it as a success.

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[*] posted on 18-4-2021 at 05:38


arkoma, what procedure did you use?
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[*] posted on 18-4-2021 at 12:56


Method 1 from this

*edit* pretty sure i would have had better yield if i had used a blender to mix the dry ingredients.

the sodium ethyl sulfate was where the learning curve kicked in, trust me. finally waited till my oil bath stabilized at 110C before i EVER set my flask/condenser/addition funnel in to it. temp in bath and internal flask both monitored (it gets warmer than this ya get diethyl either which is a side product for this procedure), slow dropwise addition of H2SO4 then reflux fer 'bout an hour. neutralized rxn mix with Na2CO3 until pH 7, suction filtered to remove the sodium sulfate (which i saved for use as dessicant), then evap'ed off the filtrate

[Edited on 4-18-2021 by arkoma]




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[*] posted on 15-8-2021 at 06:40


I maintained my oxidizer storage (which contains a few items that aren't strictly oxidizers). Most things are holding up pretty well. My bromine looks unchanged in its bottle, and the cap shows no signs of degradation. Some of my sodium dichromate is a bit clumpy. I put some additional layers of plastic around it. I also have some in a bottle with a cap that is starting to rust. I will probably look for a new bottle. There was a hole in my ammonium nitrate bag that made a bit of a mess. My mercuric chloride looked unchanged, but the foil that I used to wrap the jar that holds its bottle was visibly degraded. I put that foil in a solid waste container and rewrapped the jar then threw away the gloves and washed my hands. My chromic acid looks fine, as do my potassium permanganate, potassium dichromate, and potassium nitrate. My pool chemicals seem to be fuming a bit, but I'm not going to worry about that unless the packaging starts to degrade.

I am going to have to repackage my phosphorus oxychloride. The cap shows signs of serious degradation and probably imminent failure. I likely have a suitable bottle, but I will need to set up some sort of a fume hood.
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[*] posted on 15-8-2021 at 20:55


Quote: Originally posted by arkoma  
Method 1 from this

*edit* pretty sure i would have had better yield if i had used a blender to mix the dry ingredients.

the sodium ethyl sulfate was where the learning curve kicked in, trust me. finally waited till my oil bath stabilized at 110C before i EVER set my flask/condenser/addition funnel in to it. temp in bath and internal flask both monitored (it gets warmer than this ya get diethyl either which is a side product for this procedure)


Eh a couple of learning curves here...heating above 30C is unnecessary and above 50C is detrimental...more serious would be if the vague Rhodium directions also produce ethyl nitrite which is not mentioned; if it is expected, but trust is given to wikipedia, that it's much more volatile (by 45C) than this time-wasting project has been (maliciously) saying for the past 8 months. It would not surprise me if CA 49, 836 (1955), didn't say what Rhodium/the-hive says at all, as what it says seems to be a combination of other references, designed to give directions for none of them. I won't be the one looking it up, since the public has been completely banned from entering the local university libraries for a long time.

(edit: IIRC I looked it up over 15 years ago; the first half is from the reference CA cites but does not represent well (it's not a dry distillation there) and the second half of the "method 1" is from an earlier reference)

...on topic(?), my last project made brown oil, which can be further qualified as impure and soluble in NaOH, yet it smells exactly like safrole (after acidification). I also created smoke, coming from inside the control unit of my Buchi R110 (even though the rotation was set slow) and discovered why few of them still survive, AND confirmed that there is a good reason why Bayer's DE189843 doesn't mention yield in any way.

[Edited on 16-8-2021 by S.C. Wack]




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[*] posted on 19-8-2021 at 17:26


I opened my sodium borohydride, and I was pleased to discover that it was packaged inside multiple layers of thick foil. I had added a couple of ziplock freezer bags to that, and then abused it horribly. There was some minor clumping, but most of it is still a free-floating crystalline powder, which I put into a large glass bottle.

I am planning on getting into my sodium next, and then I'll tackle the oxidizers. I don't have a fume hood set up (I don't even have electricity yet), so I will have to use a gas mask for some of the transfers. I'm using a regular N95 mask for the powders, but I'll use an acid gas mask and probably swimming goggles for the fuming liquids.

The cleanup from sodium borohydride smells like epoxy glue, and I'm not sure why.
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[*] posted on 19-8-2021 at 17:44


What were you using to clean up the borohydride?



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[*] posted on 19-8-2021 at 19:14


Baby wipes. Ingredients: water, glycerin, pg-dimonium chloride phosphate, natural fragrances, tocopheryl acetate, sodium benzoate, citric acid. I don't have a baby here, but they were readily at hand.

I didn't have a large enough container on hand for the sodium, but I got my sodium dichromate bottled up. It was encased in five layers of plastic, and it was a bit clumpy but is free-floating after some shaking in a bottle. It might be a little damper than it should be, but I figure that's pretty normal, and I can work with that.



My bromine bottle cap is actually not looking so great now, after the bottle sat on a heated floor for a few hours. Very little bromine is missing, but it looks like there is an orange-stained crack in the cap. Fortunately, I have another cap I can use to replace it. The cap that is on it now has been there for several years.



[Edited on 20-8-2021 by JJay]
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[*] posted on 20-8-2021 at 13:26


I got my sodium under oil. I had to remove some of it from an aluminum can. The aluminum was actually pretty easy to cut, but removing the last of the sodium reminded me of scraping used chewing gum off of a cold surface wearing two pairs of gloves. I wiped down the surface, which was actually pretty exciting since there were tiny pieces of sodium scattered on it, and they burst into flame when touched by a wet cloth. Then I poured water on the fragments of the can, resulting in a fireball that burned for a minute or so while spitting fireball fragments. It went out eventually and then reignited when I poured on more water. I made sure it was not burning and completely soaked before I walked away (I'll pick up the trash later).

My bromine is chilling over ice. I am planning on just changing the cap, but I have another bottle close by with a funnel inserted if the replacement cap won't fit or something.

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[*] posted on 20-8-2021 at 13:46


The cap change for the bromine went without a hitch. I didn't even smell any bromine until I took off my gas mask. I also found a PTFE-lined cap that happened to fit on my phosphorus oxychloride bottle, so I just changed the cap. The bottle appeared to fume pretty strongly when it was open, and I didn't leave it open for long.

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[*] posted on 21-8-2021 at 10:58


Be glad to see you doing chemistry again JJay. I've been so busy traveling this year haven't done much. In Mexico for the SECOND time since May, and spent all of June in California.



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[*] posted on 21-8-2021 at 11:14


I've been cleaning up my lab in preparation for September- working syntheses that worked to various degrees.

Making a hopefully-chelating amide from methyl salicylate and en seems to have worked quite well.

Making simple amides from methyl o-toluate and methyl anthranilate did not work very well at all.

Making salicylamide worked very well, but it didn't form a simple complex with copper(II).




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[*] posted on 21-8-2021 at 13:56


Quote: Originally posted by arkoma  
Be glad to see you doing chemistry again JJay. I've been so busy traveling this year haven't done much. In Mexico for the SECOND time since May, and spent all of June in California.


I went through all of my chemicals and found a couple of leaking plastic jugs, both of which contained half-finished but fortunately non-toxic experiments that are probably ruined now. I transferred the contents to glass bottles. I reorganized all of my chemicals and most of the glassware.

I am also going to be traveling quite a bit for the next several months, but I have started preparing the site that will eventually be home to my lab. I am super tempted to take several months off and just do chemistry, but I probably shouldn't do that just yet.

I am going to do a few experiments on the road, though.

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