organicchemist25
Hazard to Others
Posts: 136
Registered: 12-2-2014
Member Is Offline
Mood: No Mood
|
|
Nitrotoluene question
I attempted making nitrotoluene last night. I have a question. Is there supposed to be a dark top layer? The procedure mentions nothing of it, in
fact, it says two separate yellow layers. If, it is not likely, what might I have?
I freshly made nitric acid (conc H2SO4 and KNO3) the night before. It is concentrated. It always has the highlighter yellow tint when I make it. It
reacts strongly with Cu. I actually need to add a couple drops of water to initiate the reaction. I also boiled down approx 40% battery acid from the
auto store until the H2SO4 is thick and smoking thick white smoke, so I know that is about as concentrated as I can get.
I even freshly distilled my toluene over a small piece of sodium.
Any ideas?
Oh, and, the reaction (i had in crushed ice bath with copious amounts of NaCl) and the temp NEVER went above 7-8 C. I expected some exothermic
activity. The thermometer never even increased as I added about 2-3 ml every minute or so. I kept a good eye on the temp. no increase in temp during
the entire reaction.
I could notice that it was changing color as the reaction progressed. The initial solution was pretty clear. I could see the stir bar and vortex for
a while. After no temp increase for some hours, i felt it was safe to go to bed. I left it stirring all night. This morning it has a dark, distinct
layer.
Any and all help would be greatly appreciated.
[Edited on 27-7-2014 by organicchemist25]
|
|
Mailinmypocket
International Hazard
Posts: 1351
Registered: 12-5-2011
Member Is Offline
Mood: No Mood
|
|
Have you had a read over Magpies very nice write up on this?
http://www.sciencemadness.org/talk/viewthread.php?tid=29111
Might be helpful visually
|
|
organicchemist25
Hazard to Others
Posts: 136
Registered: 12-2-2014
Member Is Offline
Mood: No Mood
|
|
No, I had not. Thank you and thanks for supplying the link, as well!
|
|
S.C. Wack
bibliomaster
Posts: 2419
Registered: 7-5-2004
Location: Cornworld, Central USA
Member Is Offline
Mood: Enhanced
|
|
Dilute NaOH washes. Nitrotoluene is never run cold AFAIK, sounds like you might be using some weird directions.
|
|
Chemosynthesis
International Hazard
Posts: 1071
Registered: 26-9-2013
Member Is Offline
Mood: No Mood
|
|
^ Always best to cite your procedures, as required when publishing peer-reviewed literature, for help.
It helps us understand any methodological flaws and optimize your procedure.
|
|
organicchemist25
Hazard to Others
Posts: 136
Registered: 12-2-2014
Member Is Offline
Mood: No Mood
|
|
Will do, from here on out. Definitely doing Magpies write-up.
Thank you for all the replies
|
|