Oops wrote the name slightly wrong if trying to stay consistent with the way the paper(at bottom) did names. Should be "3F-2CL-DPPy. Reddit won't let me edit title.
For those who are not familiar, this is related to the nmda antagonists ephenidine, fluorolintane, and others.
250 mL of THF, 1.9mL of TFA, and 12.9 grams of zinc dust were added to a round bottom flask under argon.
24.2mL of 3F-benzyl bromide was added slowly. (My God is this a potent lachrymator.)
After cooling down, 9.1mL of pyrrolidine and 11.1mL of 2CL-benzaldehyde were added and the mixture was left to stir for 24 hours at room temperature under argon.
Upon completion the reaction was quenched with 70mL of hcl acid in 300mL of deionized water. Reaction mixture was extracted with 175ml of 60/40 heptane/ethyl acetate twice to remove organic impurities. A small amount of hcl and water was mixed with the organic impurity layer to extract any last little bit of amine. This was combined with aqueous layer.
Also one thing to note is that strangely when I first mixed the aqueous and organic I noticed 3 layers formed(the thf must of been salted out previously from zinc and amine salts). I added some water to see which layer was the aqueous one and to my surprise all of a sudden a crap ton of white precipitate started crashing out and the thf layer disappeared. So I decided to filter the precipitate assuming it was the product and zinc chloride.
Then I added ammonia and water to the precipitate and extracted the product with 60/40 heptane/ethyl acetate. The product is distilling now to dryness to remove any left over pyrrolidine.
I will later attempt to add base to the aqueous/thf layer, extract that with 60/40 Hep/Ethyl, and then distill just in case there is still some product leftover. Then I will add a small amount of heptane to the distillate, combine both, dry with magnesium sulfate, bubble hcl gas, filter, wash with cold heptane, and dry to hopefully have the pure product.
If anyone is interested these are the affinities from the paper where they made a load of 1,2-diarylethylamines(some very similar) and tested their affinities.
https://imgur.com/a/1-2-diarylethylamine-affinities-MHFOKqE
This paper is where I got the procedure and the idea for the modified mannich barbier.
Check out r/nervewing 's post(contains links to the paper and everything.)
https://www.reddit.com/r/dissociatives/s/U1J4BwihXs
Also, if anyone has any pharmacological intuition as to the activity of this compound, guesses are appreciated!