The reason I ask is that it is a new message, stating chemicals can not be shipped to residential addresses. I have ordered many times before from them, the message was never there. I'm wondering if it's to cover their asses, but if individual ordering is still an option.
Also, I recommend a reduction of all halogentated/alkyl substituted nitrostyrenes using sodium borohydride/zn one pot, info can be found on PEA thread in hyperlab. great yields, clean reaction. I can say that with proper equipment and chemicals you can go from 4-methoxyphenol to 2,5-dimethoxyphenethylamine easily. The hardest part is methylation but I recommend you make the potassium salt of 2-hydroxy-5-methoxybenzaldehyde in EtOH, then after filtering and briefly sucking dry, heat with 2 eq TMP in a boiling water bath, the salt disappears and although my notes aren't handy, few hours I believe reaction was over. All preparation of the salt must be done quickly as it oxidizes in air. This gives about 60% yields, I've done it and it works. Bisulfite purification is always necessary.
Also do not disregard the magic of benzoquinone/thiourea, if you don't know what I'm talking about check SM a wide variety of substitute PEA and 4-thioPEA can be made, formylation is done differently though once again info is on hyperlab. The 2c series has been my area of interest for a while and I'm telling you it's so OTC except for some things but these things are not hard to buy on the net, nor are they suspicious.
Ok well anyway, I must say that mg formylation With paraformaldehyde is the ONLY way to formylate the phenol, do not waste your reagents with the chloroform bullshit. With the mg yu end up with more aldehyde than penol begun with, 90+ yield is obtainable easily. And you need this, because methylation is the main loss in yields overall. Even with access to DMS, yields aren't that great and are not very reproducible.
I've tried methylation of the salicylaldehyde in DMF/KOH/TMP and DMF/K2CO3/TMP but it's a dirty and not very well yielding reaction. About 40% and it's very dirty. Take the time making k salt, heat, much nicer.
Something i have not tried yet but am very eager to is simple bromination of 1,4-dimethoxybenzene, info is available somewhere on the net, it's otc. Then formylation with duff using the improved method.
Zinc reduction of 2,5-DMNS is probably the most OTC,cost effective and good yielding reduction method available as I'm sure you all know. But it can't be used for all nitrostyrenes as unhalogenated products and other crap happens, so borohydride/zn is great, also al/hg will work for many. Because 2c-x should not be our only goal! So many PEA can be made its ridiculous. Get precursors while you can!
looks like one can skip the methylation step now and move straight to reimer formylation then to the nitromethane reaction and reduction and on to halogenation. The problem now is handling nitromethane.
