Please do not xpect much from this..... Jerry (that's his Russian pseudonym - a friend of Assholium's, BTW
) was very very sparse, as usual - those pro's, damn 'em!
Anyway, here goes a verbatim transcryption of his notes:
1. In a 2-liter flask w/a gas absorption tube there are placed 64 g p-diMeO-benzene in 300 ml benzene and added ~30 g wet paraform (filtered from polymerized on standing formaline) and a stream of HCl is passed for 1,5 h. The precipitate is filtered through cottonwool. Filtrate is shaken twice w/cold water in a sepfunnel. Dried w/anh K2CO3 and evap off the benzene. The product crystallizes on standing (mp=69 C, lit. = 72 C). The obtained crude product is distilled in vacuo. Yield 16,3 g.
2. In a 150 ml flask there are dissolved 16 g of the above product in 60 ml acetone. Added 8 g KCN and 0,8 g NaI and refluxed for 24 h. The precip't't is filtered and washed w/acetone. After evap'n in vacuum there is left 7,2 g brown oil that crystallizes on standing.
3. For red'n of the bulk of the above crude product one takes 5 g LAH in 250 ml ether and treats as usual.
- see #20 (2C-B) in PiHKAL.
- 1 g of the product is obtained
- the product differs from the expected 4-bromo-2,5-diMeO-phenethylamine (!!)
- possibly, contains some 1,4-bis-(2-aminoethyl)-2,5-diMeO-benzene.
I know that's not much - esp, details of bromination are missing. But i still think that's of significant value, since - while the yields are low, of course - that's the 1st known success w/chloromethylation of p-DMB - whatever the result might bee.
As you can see, Jerry wasn't particularly anal about purification of intermediates
He's generally like that
Some additional info - the activity range, e.g. - can bee found in
Post 15822 (missing)
(C_Nemo: "Re: chloromethylation/formylationof 2,5-diMeO-somethin", Chemistry Discourse).
Antoncho