Author Topic: Roads to Nitroethane  (Read 6805 times)

0 Members and 1 Guest are viewing this topic.

Hansje

  • Guest
Re: Roads to Nitroethane
« Reply #20 on: February 23, 2001, 11:55:00 AM »

provided that DCM and nitroethane doesn't form an azeotrope


This came from some azeotrope didicated webpage:
Binary azeotropes of:
(substance/bp/comp.wt%-wt%)
Nitroethane:
1-butanol/107.7/55-45
toluene/106.2/25-75
DCM:
glycol/168.7/86-14

They don't claim to list all existing azeotropes, but they list so many that I don't think DCM/nitroethane will form one.



Hansje Pansje Kevertje.....

Rhodium

  • Guest
EtOH/HCl/ACOH/NaNO2 nitroethane method disproven
« Reply #21 on: April 08, 2002, 07:55:00 PM »

otto

  • Guest
doesn't work
« Reply #22 on: April 08, 2002, 09:23:00 PM »
hi ab2,

don't bee angry on otto, but it seems that all your effort was useless. check out Synlett; 07, 2001, pp 1121-1122 the article "Can Nitroalkanes be Obtained Directly from Alcohols and Sodium Nitrite in Acetic Acid - Hydrochloric Acid Mixture?" says that it isnt possible, instead of nitroalkanes they always got the corresponding nitrite esters. you can get the .pdf from www.thieme-connect.com, when you sign a trial-account.

otto

Rhodium

  • Guest
Letters
« Reply #23 on: April 08, 2002, 09:42:00 PM »
Otto: Uh? I have uploaded exactly that PDF to my website above.

Aurelius

  • Guest
Doesn't Work?
« Reply #24 on: April 09, 2002, 02:03:00 AM »
Hey Rhodium, "this method is history..."  are you saying that it doesn't work?

Rhodium

  • Guest
Does not work
« Reply #25 on: April 09, 2002, 02:18:00 PM »
Yes, and why it is so is detailed in the PDF file I linked to (it is the PDF version of the article otto refereced).

Aurelius

  • Guest
Isomerization
« Reply #26 on: April 10, 2002, 12:04:00 AM »
So, if we can in good yeild produce ethyl nitrite- why not?  It is easy enough to convert to nitroethane by isomerization, right?

https://www.thevespiary.org/rhodium/Rhodium/chemistry/nitrite2nitro.html



didn't read the whole thing, so if there is a reason that this is hard to do, please state. 


Rhodium

  • Guest
Nitrite 2 nitro
« Reply #27 on: April 10, 2002, 01:36:00 AM »
It is much easier to produce ethyl nitrite than using the method described in the article, just look at my page - ethanol, NaNO2 and H2SO4 - no need for DCM/HOAc.

The isomerization method is indeed theoretically easy, but not suitable on a small scale.

Aurelius

  • Guest
Minimal size
« Reply #28 on: April 10, 2002, 05:59:00 AM »
So what do you think the minimal size would be?  and how to make it "safe".

Aurelius

  • Guest
Read the Article
« Reply #29 on: April 10, 2002, 06:10:00 AM »
Rhodium, as is the usual case, is correct.  the percent yeild really isn't that bad (10% of nitroethane by volume) considering the recycling for repeated attempts for converting the rest of the nitrite.  However, the article stated that it took 4-5 HOURS to pass a relatively small (less than a liter) of nitrite through.  if one had a continuous still (dangerous) aurelius could see the benifit.  But as Rhodium stated- not for small scale.

Aurelius

  • Guest
Routes to Nitroethane
« Reply #30 on: April 10, 2002, 06:16:00 AM »
Just thought it was appropriate

Post 238118

(Aurelius: "Re: What can be done to improve the performance of clandestine nitroethane synth?", Chemistry Discourse)

ChemicalSolution

  • Guest
etNO2 from etBr in DMSO
« Reply #31 on: April 10, 2002, 06:28:00 AM »
SWIM did 3 batches of this stuff...  All of her distilled products had a density of around 2g/ml.. She vac distilled, distilled @ 1ATM, and lastly, distilled with water..  Any other bees (that bothered to mass the distillate) have this problem??

otto

  • Guest
ups
« Reply #32 on: April 11, 2002, 12:17:00 AM »
hi rhodium,

before otto started to type your post wasnt there. then some people came in drawing otto off the computer for a talk and otto of course didnt check again the forum before finishing the post.

otto