Sciencemadness Discussion Board

Aniline in Beaker

DFliyerz - 3-8-2015 at 16:53

Recently I finished preparing a nice batch of nitrobenzene from benzene and am planning to reduce it to aniline, but ran into a problem where the only video I've seen on the process uses a lot of equipment that I don't have like a mechanical stirrer and a three-neck RBF. I'm wondering; can this procedure be done in a beaker with hand-stirring with a glass rod?

ParadoxChem126 - 3-8-2015 at 19:03

In theory it may be feasible to perform this reaction in a beaker with hand stirring, but ultimately the reaction yield would be poor. Without sufficient agitation, the reaction rate is considerably slower, and complete conversion to aniline is unlikely in a reasonable amount of time. An overhead stirrer is the best way to achieve adequate mixing.

On a side note, the reaction you plan to execute requires a steam distillation. For these distillations, a two or three-neck round bottom flask is typically employed as the main distillation flask (steam comes in one side and the vapor mixture leaves the other). However, a single-neck flask can also be used when coupled with a Claisen adapter. What do you plan to use as a distillation vessel?

[Edited on 8-4-2015 by ParadoxChem126]

DFliyerz - 3-8-2015 at 19:27

I plan to do a steam distillation by simply adding water to the flask and mixing it thoroughly while distilling.

ParadoxChem126 - 3-8-2015 at 19:30

You will need a fairly large flask to contain the entire reaction mixture in addition to the extra water required to generate steam.

DFliyerz - 3-8-2015 at 19:43

Quote: Originally posted by ParadoxChem126  
You will need a fairly large flask to contain the entire reaction mixture in addition to the extra water required to generate steam.


Well, my largest RBF is 500ml and my largest beaker and Erlenmeyer are 1000ml, but I can just scale everything down.

ParadoxChem126 - 3-8-2015 at 20:24

You can always position an addition funnel at the top of the still head to add more water as it is distilled away.