I did this for my own notes. A damn shame it worked poorly. I'm going to attempt to scrutinize it. I suspect that the steam distillation tainted it and it seems unnecessary anyway
I did this for my own notes. A damn shame it worked poorly. I'm going to attempt to scrutinize it. I suspect that the steam distillation tainted it and it seems unnecessary anyway
There is new video about P2NP synthsis by henry reaction with very good details on Youtube By TDC.
I cant post the link. It might be again the forum rule
There is new video about P2NP synthsis by henry reaction with very good details on Youtube By TDC.
I cant post the link. It might be again the forum rule
This is the detailed method.
You can find details from Uncle fester book 8th edition meth manufacture, page 68.
I pasted that relevant section.
"
The following variation of the Knoevenagel reaction will give higher yields of product than the first
method. The reason for the higher yield is the use in this method of toluene as solvent, and the placement
of a Dean Stark trap above the t1ask to remove water from the mixture as it is formed. Removal of water
favors the formation of greater quantities of nitroalkene.
To do the reaction, a 1 000 ml round bottom flask is filled, in this order, with 200 ml of toluene, 1 00 ml
of benzaldehyde, 90 grams (86 ml) of nitroethane, and 20 ml of butylamine. It is a good idea to swirl the
flask after adding each ingredient to prevent layers from forming. Next the t1ask is placed on a one
burner electric buffet range with infinite control, and the glassware is set up as shown in Figure.
The Dean Stark trap is attached to the flask, and a condenser is attached to the Dean Stark trap. Then
the butTet range is turned on at a heat setting high enough to produce a rapid boiling of the toluene, and
cold water is flowed through the condenser. As the reaction is progressing, the vapors of toluene carry
water along with them, and when they tum back to liquids in the condenser, the water will settle in the
trap portion of the Dean Stark trap because water is heavier than toluene. You will also note a milky
appearance to the toluene due to suspended water in it. The trap portion of the Dean Stark trap is
graduated in milliliters. This allows you to keep track of how much water has been collected. Half of the
water is collected in the first hour, and the full amount ( 1 8 ml) is collected after five hours of boiling.
When this is done, the heat is removed, and the flask allowed to cool. This phase of the reaction has j ust
made the nitroalkene. I f one should wish to collect the nitroalkene for direct reduction to amphetamine.
one just needs to remove the Dean Stark trap, rig the flask for simple distillation as shown in Figure I I ,
and remove the toluene under a vacuum from an aspirator."
