First Attempt at 2C-N Synthesis (Procedure in Post)
First Attempt At 2C-N Synthesis
Procedure:
Into a beaker equipped with a thermometer, 1g of 2C-H freebase was dissolved into 20mL of GAA in a cold water bath. Under heavy stirring 3.3mL of azeotropic nitric acid was slowly added from a pipette. No sudden temperature spike was noted and a temperature of 19-21C was maintained during the entire addition.
The mixture was left stirring for one hour after the addition of nitric acid, but no 2C-N nitrate precipitated. After trying some methods to get crystals to form, it was found that after heating the solution to 100C (over which time the volume of the solution reduced by 2mL) and then placing it into the freezer caused yellow crystals of 2C-N to precipitate.
The solution was filtered while cold and washed with DCM (this was a mistake, as the nitrate salt of 2C-N appears to be somewhat soluble in DCM)
Conclusions and Improvements:
After drying there remained 0.3g of the powdery yellow nitrate salt, representing a measly 19% yield. I’m not entirely sure why the yield was so low aside from the mistake with the DCM. But I have a couple guesses. If I were to redo this, which I likely will, I would approach it slightly differently. I would like to try using less GAA, keeping the solution colder during the nitration, and adding 20% NaOH solution after the reaction has completed until it’s strongly basic instead of precipitating the nitrate salt. From there going on to extract the freebase and doing a regular work up, probably opting to precipitate the HCl salt.
