yourawesomesauce67
infraorbidal
- Joined
- Mar 3, 2026
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So to people who have been tracking my threads, i decided to make this compound myself from aspirin.
I started by extracting the aspirin from tablets using 91% isopropyl alcohol, but the water content caused some hydrolysis and I lost a lot of material during filtration, dropping my yield to around approximately 65%(I think)
I converted the aspirin to salicylic acid by boiling it with hydrochloric acid, then distilled it to phenol, though I think the setup caused a vapor leak and I definitely did not redistill it for purity.
I nitrated the phenol with nitric acid but something caused the temperature to spike which produced some side products. (Added too fast maybe?)
After both purification and precipitation with hydrochloric acid,I recrystallized from ethanol and I put it in the freezer instead of letting it cool slowly.
The freezing caused the compound to precipitate as microcrystals,
I THEN tested the meltingpoint and got 106-109 degrees C, which is close to the literature value of 108.5 but slightly depressed and widened, which should indicate about 88% purity with some residual solvent and minor nitration isomers present.
The bright yellow color seems to confirms the correct chromophore is intact,and I did not dry it completely because the dry compound is shock sensitive and can detonate,(literally dnp was used as an explosive lol)
so I left it slightly damp with residual ethanol, which is why it came out sort of clumpy
Here are results, i already contacted my local my local EHS department for pickup, as you can’t simply just throw this in the trash or down the drain( as again, it’ll explode)
What I tried to go for:
I started by extracting the aspirin from tablets using 91% isopropyl alcohol, but the water content caused some hydrolysis and I lost a lot of material during filtration, dropping my yield to around approximately 65%(I think)
I converted the aspirin to salicylic acid by boiling it with hydrochloric acid, then distilled it to phenol, though I think the setup caused a vapor leak and I definitely did not redistill it for purity.
I nitrated the phenol with nitric acid but something caused the temperature to spike which produced some side products. (Added too fast maybe?)
After both purification and precipitation with hydrochloric acid,I recrystallized from ethanol and I put it in the freezer instead of letting it cool slowly.
The freezing caused the compound to precipitate as microcrystals,
I THEN tested the meltingpoint and got 106-109 degrees C, which is close to the literature value of 108.5 but slightly depressed and widened, which should indicate about 88% purity with some residual solvent and minor nitration isomers present.
The bright yellow color seems to confirms the correct chromophore is intact,and I did not dry it completely because the dry compound is shock sensitive and can detonate,(literally dnp was used as an explosive lol)
so I left it slightly damp with residual ethanol, which is why it came out sort of clumpy
Here are results, i already contacted my local my local EHS department for pickup, as you can’t simply just throw this in the trash or down the drain( as again, it’ll explode)
What I tried to go for:
