reflux apparatus (rubber stopper in 3 neck flask which i do not have an adapter for) sprung a leak.. ie cork poped out while i was having a smoke outside (i know... stupid ass newbie fuck leaving first time reaction alone!) and the dcm quickly distilled off and mix got up to about 95C)
A "fixed cork" is not a "reflux apparatus".
Here is a picture of a reflux apparatus:
(https://www.thevespiary.org/rhodium/Rhodium/hive/hiveboard/picproxie_docs/000531022-file_lfsk.jpg)
Breathing DCM fumes can KILL YOU.
Inhalation - Dizziness. Drowsiness. Headache. Nausea. Weakness. Unconsciousness. Death.
http://www.cdc.gov/niosh/ipcsneng/neng0058.html (http://www.cdc.gov/niosh/ipcsneng/neng0058.html)
Peracids can EXPLODE when heated to 110 Celcius and over.
Flammability and Explosibility Peracetic acid explodes when heated to 110 °C, and the pure compound is extremely shock sensitive. Virtually all peracids are strong oxidizing agents and decompose explosively on heating. Moreover, most peracids are highly flammable and can accelerate the combustion of other flammable materials if present in a fire. Fires involving peracetic acid can be fought with water, dry chemical, or halon extinguishers. Containers of peracetic acid heated in a fire may explode.
http://www.hhmi.org/research/labsafe/lcss/lcss68.html (http://www.hhmi.org/research/labsafe/lcss/lcss68.html)
i quickly cooled it down to about 60C and added dcm so it was refluxing smoothly thru the rest of second addition of performic.
How was it refluxing? DCM has a boiling point of 39 Celcius, so without some type of condensing, it would have evaporated into the atmosphere again.
Did you have all the necks sealed?
especially the glycol. as per abolt's reply, after distilling dcm for 2 hours, i added weak vaccuum and about 30mls more came over. i set dcm aside to see if the 30mls was really dcm. the glycol at room temp was almost blak and thick like honey, was slightly red when held up to light. here was a very clear difference.
You have toasted your reaction.
did a bisulfite test and the whloe tube crystallized with some fatty shit on top. i guess my question is... is bisulfite test enough to ensure that i have mdp2p or could it still be some other ketone?
I would be surprised if you had anything useful. UTFSE for the words "chicken fat".
Dude, don't take this the wrong way, but you have at least several months more reading to do. Please don't kill yourself.