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Turner
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[*] posted on 23-8-2014 at 07:39


It's not interesting at all to make an ANNMAL cap, not to mention terribly unreliable. No, there's zero chance of it detonating from pressing it. RDX is probably the least sensitive material I would ever use in a detonator.





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[*] posted on 23-8-2014 at 08:42


Quote: Originally posted by Turner  
It's not interesting at all to make an ANNMAL cap, not to mention terribly unreliable. No, there's zero chance of it detonating from pressing it. RDX is probably the least sensitive material I would ever use in a detonator.

For me, it seems interesting since it allows to make a detonator safely at the last moment and 0.2g SADS can't do damages or very little.
The guy in the video was exploding 20g to more 100g boosters of activated ANNMAL directly with a single cap 200mg SADS.

Why you said "No, there's zero chance of it detonating from pressing it"? for what reasons then.. because i think this guy already made it




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[*] posted on 23-8-2014 at 19:32


I doubt it would work as you will have problems with critical diameter in a 1ml syringe. pressing ANNMAL is not likely to make it detonate. Also very small AN charges may not even detonate at all especially when pressed. The only other way is to give it a try.



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[*] posted on 27-8-2014 at 20:58


Quote: Originally posted by hyfalcon  
They also sell DampRid which is pure calcium chloride at most home stores.


Bit of a thead necro, but I just wanted to note that DampRid, despite its MSDS and labeling, contains some single digit percentage of some impurity. Probably irrelevant if you're just using it to dry something, but for metathesis reactions it may cause issues. I tried to synthesize 2 moles of CuCl2 via CuSO4 + CaCl2 (as DampRid), with followup addition of a small amount of oxalic acid to clear the remaining CaSO4 from solution. But boiling down precipitated several grams of an additional white substance that formed fibrous crystals. I'm guessing this is some anti-caking agent that is added to stop the DampRid from clumping. Not a showstopper but if you really want 99+% pure CaCl2 you should use something else.




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[*] posted on 29-8-2014 at 10:21


@bbartlog,
So if I do understand correctly:
CuSO4 + CaCl2 --> Cu(2+) + 2Cl(-) + CaSO4(s)

But
CaSO4 <==--> Ca(2+) + SO4(2-) (at ambiant T° solubility is > 15g/L)

then you try adding oxalic acid to precipitate Ca oxalate and generate sulfuric acid...
HO2C-CO2H <==> 2H(+) + (-)O2C-CO2(-)
Ca(2+) + (-)O2C-CO2(-) <--==> Ca(C2O4)(s)
2H(+) + SO4(2-) <==> H2SO4

The problem is antagonist equilibriums...
H2SO4 is way stronger acid than oxalic.
Ca oxalate is weakly soluble much more than Ca sulfate.

So probably you get intermediate reactions because H2SO4 dissolution (acidity) forces oxalic acid to be present as the molecular species and not as the dianion.

Or you get a weird intermediary system with CaHSO4 and Ca(O2C-CO2H)2 because both H2SO4 and HO2C-CO2H are diacids...

[Edited on 29-8-2014 by PHILOU Zrealone]




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[*] posted on 29-8-2014 at 17:59


Quote: Originally posted by bbartlog  
Quote: Originally posted by hyfalcon  
They also sell DampRid which is pure calcium chloride at most home stores.


Bit of a thead necro, but I just wanted to note that DampRid, despite its MSDS and labeling, contains some single digit percentage of some impurity. Probably irrelevant if you're just using it to dry something, but for metathesis reactions it may cause issues.


Indeed!

Calcium chloride is a common garden soil supplement, used by gardeners & vegetable growers after heavy rains deplete soil of available Ca... Which can cause your tomato/pepper/squash plants to develop "Blossom End Rot"

Last year, I thought the same thing... Damp rid, which I had on hand, must be pure CaCl and would be just the thing to use when my garden plants showed signs of Ca shortage after a series of heavy rains.

Whatever the other chemical(s) in DampRid may be, they are not very water soluble. A whitish blanket of undissolved material remained after dissolving most of the DampRid in hot water, decanted the solution from this and used it anyhow. Didn't hurt my tomato and pepper plants, but I will buy garden supplement grade or ice melter grade calcium chloride for either chemistry or garden use in the future.




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[*] posted on 6-11-2014 at 06:58


I just found an MSDS for the Damprid brand moisture absorbers and in the composition/information on ingredients section it states:

1. Calcium chloride 60.00-100.00%
2. Sodium chloride 1.0%-5.0%
3. Potassium chloride 1.0%-5.0%

Shame they can't give you exact percentages. But this doesn't clear up the fact that the additional chem's added are not water soluble because obviously both Potassium chloride and Sodium chloride are.
Is there something else added they don't mention?


[Edited on 6-11-2014 by greenlight]



[Edited on 6-11-2014 by greenlight]
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[*] posted on 6-11-2014 at 08:08


There is an anti cakeing chemical added, as noted above.

There is also a formulation with scent added, I'd avoid that product.




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[*] posted on 7-11-2014 at 02:26


just a quick question
could you make meta nitro benzoic acid by treating nitrobenzene with phosgene in the presence of catalysts like AlCl3 or glacial acetic acid(they use acetic acid while brominating the ring to activate the bromine) and hydrolysing it

[Edited on 7-11-2014 by CuReUS]
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[*] posted on 7-11-2014 at 05:53


Why not just nitrate benzoic acid? The meta product will be predominant.




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[*] posted on 7-11-2014 at 09:48


actually i came across this in my lab record from my undergrad days .i think we had a synthesis challenge at the end of the term and our teacher had given us nitrobenzene as the starting product.What i ended up doing back then was another nitration to get meta dinitro benzene which i selectively reduced using NH4HS to get meta nitro aniline ,which i diazotised and treated with CuCN to get meta nitro benzonitrile which i finally hydrolysed to get meta nitro benzoic acid

looking back i think if you could just treat it with phosgene ,my work would have been much easier ( and i might have won the prize:( ) .IIRC ,the guy who ended up winning used a grignard approach.

also nitrating benzoic acid is not a good idea because of the deactivating nature of the COOH group
see this http://webcache.googleusercontent.com/search?q=cache:XI5fQ0f...

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[*] posted on 7-11-2014 at 13:57


IMHO a Grignard approach is usually indicated when making an aromatic acid barring other factors of course. Yield is usually excellent and the reactions are easy to run.



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[*] posted on 7-11-2014 at 15:46


Quote: Originally posted by CuReUS  

also nitrating benzoic acid is not a good idea because of the deactivating nature of the COOH group
see this http://webcache.googleusercontent.com/search?q=cache:XI5fQ0f...



In my organic chemistry class we nitrated methyl benzoate to methyl m-nitrobenzoate. I can't imagine the acid to be much harder to nitrate than the methyl ester.




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[*] posted on 7-11-2014 at 21:57


Quote: Originally posted by chemrox  
IMHO a Grignard approach is usually indicated when making an aromatic acid barring other factors of course. Yield is usually excellent and the reactions are easy to run.
Quote: Originally posted by Cheddite Cheese  
Quote: Originally posted by CuReUS  

also nitrating benzoic acid is not a good idea because of the deactivating nature of the COOH group
see this http://webcache.googleusercontent.com/search?q=cache:XI5fQ0f...



In my organic chemistry class we nitrated methyl benzoate to methyl m-nitrobenzoate. I can't imagine the acid to be much harder to nitrate than the methyl ester.


chemrox-but aren't aromatic grignards very difficult to initiate
during my undergrad ,we once made phenyl magnesium bromide so that we could react it with methyl benzoate to make triphenylmethanol
we spent almost 45 minutes trying to react the magnesium with bromobenzene by scratching the magnesium at the bottom of the flask as our teacher had instructed
some people even made a hole through their flask and the magnesium ignited and caused quite a chaos that day

but the guy who won was damn smart:mad:
he used ethane 1,2 dibromide as an initiator to kick start the reaction ,and it worked like a charm.
maybe it was also because of the withdrawing nature of the nitro group:o

cheddite-the orsyn page that i linked uses methyl benzoate as the starting material .maybe the ester is a lesser deactivating group than the acid
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[*] posted on 8-11-2014 at 05:42


In my organic class, we also made triphenylmethanol, but from benzophenone and the Grignard reagent. The phenylmagnesium bromide formation went easily. We ground up the magnesium metal immediately before adding it to the reaction mixture.

[Edited on 8-11-2014 by Cheddite Cheese]




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[*] posted on 8-11-2014 at 06:31


Quote: Originally posted by Cheddite Cheese  
We ground up the magnesium metal immediately before adding it to the reaction mixture.


IIRC ,we used magnesium turnings for the reaction.
but dont you think using Mg powder or dust would be dangerous ,considering that metal dusts form explosive mixtures with air and there is copious amounts of ether around to add fuel to the fire:o
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[*] posted on 13-11-2014 at 08:14


Grignard with a nitroaromatic?
Would'nt the nitro group be reduced by the Mg into Ar-N=O, Ar-NH-OH, Ar-N=N(O)-Ar, Ar-N=N-Ar or Ar-NH2?




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[*] posted on 14-11-2014 at 08:37


About the activation of the Mg towards aromatic halide for Grignard's reaction, one may also use a tiny I2 cristal.

About the activation by Br-CH2-CH2-Br...it may react via an unwished Wurtz coupling pathway or dehalogenation...
Ar-Mg-Br + Br-CH2-CH2-Br --> Ar-CH2-CH2-Br + Ar-CH2-CH2-CH2-CH2-Ar + MgBr2
Br-CH2-CH2-Br -Mg/ether-> Br-CH2-CH2-CH2-CH2-Br + (-CH2-CH2-)2 + (-CH2-CH2-)n + CH2=CH2 + MgBr2

[Edited on 14-11-2014 by PHILOU Zrealone]




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[*] posted on 15-11-2014 at 20:27


Quote: Originally posted by PHILOU Zrealone  
Grignard with a nitroaromatic?
Would'nt the nitro group be reduced by the Mg into Ar-N=O, Ar-NH-OH, Ar-N=N(O)-Ar, Ar-N=N-Ar or Ar-NH2?


this is quite interesting ,i didn't know that grignards could act as reducing agents

BTW,treating nitrobenzene with phosgene followed by subsequent hydrolysis works ,i checked it out:D
good yield of meta nitro benzoic acid is obtained ,although there is a little coupling as well;)
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[*] posted on 25-11-2014 at 07:10


I was always taught that deactivation only really becomes an issue after two deactivators on a ring.
Contrary to what some may have been led to believe, nitration of benzoic acid is commonplace, and there is a qualitative test based on it (Mohler's test).
In fact, dinitration is possible without complication (PMCID: PMC1197580 Biochem J. Oct 1951; 49(5): 700–704.)
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[*] posted on 25-11-2014 at 22:22


Quote: Originally posted by Chemosynthesis  
I was always taught that deactivation only really becomes an issue after two deactivators on a ring.


but i remember that one of my friends from that undergrad batch tried a friedel craft alkylation of nitrobenzene followed by KMnO4 oxidation for getting meta nitro benzoic acid

she was ecstactic that she had worked out the shortest route among all of us (the grignard guy was sceptical though :mad: )

sure enough ,she failed miserably and became the butt of all jokes for the remaining term :( :(
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[*] posted on 26-11-2014 at 07:33


Quote: Originally posted by CuReUS  
Quote: Originally posted by Chemosynthesis  
I was always taught that deactivation only really becomes an issue after two deactivators on a ring.


but i remember that one of my friends from that undergrad batch tried a friedel craft alkylation of nitrobenzene followed by KMnO4 oxidation for getting meta nitro benzoic acid

she was ecstactic that she had worked out the shortest route among all of us (the grignard guy was sceptical though :mad: )

sure enough ,she failed miserably and became the butt of all jokes for the remaining term :( :(

You are comparing two very different things here. First, the theory means nothing without the data. You can apply the theory or extrapolate from a named reaction to a new substrate and impress a professor in lecture, but fail miserably to get a lab result due to the most substrate-specific molecular quirks.

The way this is often taught is that the nitronium ion is a very strong, rich electrophile relatively speaking. Nitration of bromobenzene, dinitration of benzene, FC alkylation of polybenzenes, and similarly deactivated benzenes (not nitro) have been reported in literature, to further support the notion that deactivation is a guideline rather than a rule (the first being a common undergraduate laboratory procedure in years past).

Contrast with FC acylation, for example, which often gives only or predominantly one acylation of benzene due to deactivation. It sort of makes sense that having the electron deficient Lewis acid catalyzed EAS alkylation mechanism work on a similarly deactivated benzene would fail.
The specifics get interesting: DOI: 10.1021/jo00299a051
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[*] posted on 13-12-2014 at 15:19


https://www.youtube.com/watch?v=RdYtd0rxxYk

I just wanted to post this video, beautiful effect of the explosive, looks like TNT.
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[*] posted on 21-12-2014 at 08:51


Hi

Does anyone have a synthesis for ETN using 95%< HNO3 + 95%H2SO4+ eritrol ?

I have a lot of synthesis pdfs for ETN, but they all just uses nitrate salts/65%HNO3+H2SO4
I dont think that i want to make it that way, cause i have enough RFNA atm and dont want to have a (partly) underitrated yield

Vlad

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[*] posted on 21-12-2014 at 09:30


I have tried ETN synthesis with anhydrous nitric acid and sulfuric acid a few times and I am still not sure why but I could never get above 60% yields with any process.

This describes a synthesis of ETN with pure nitric and sulfuric acids:

http://energetics.chm.uri.edu/system/files/ETN%20Paper%20acc...
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