Post 208279 (https://www.thevespiary.org/talk/index.php?topic=12230.msg20827900#msg20827900)
(Antoncho: "Re: An easy OTC 2,5-diMeO-phenylmercaptan", Novel Discourse)).Post 208025 (https://www.thevespiary.org/talk/index.php?topic=12230.msg20802500#msg20802500)
(Antoncho: "Preparation of S2Cl2", Novel Discourse) &Post 208077 (https://www.thevespiary.org/talk/index.php?topic=12230.msg20807700#msg20807700)
(catastrophe: "Re: Preparation of S2Cl2", Novel Discourse) just at higher temps.Post 229993 (https://www.thevespiary.org/talk/index.php?topic=6597.msg22999300#msg22999300)
(foxy2: "Acetyl Chloride/Acid chloride production!", Chemistry Discourse) some patents were described for methyl substituted aromatic acid chlorides but nothing on methoxy versions.http://www.webelements.com/webelements/elements/text/S/chem.html (http://www.webelements.com/webelements/elements/text/S/chem.html)
Ah Antoncho! I was hoping you or Catastrophe would show up since you've both got some practical knowledge of dabbling with these dark compounds!
:) Me, hardly at all :) I wonder where Catastrophee is now ...
You see, SWIM nearly killed himself a coupla times trying to make smth. that could bee substituted for POCl3 in Vilsmeier formylation. So now he's really elated about finding such a simple one-pot way to make SOCl2.
One-pot it is. You just make SCl2 from S (no need for S2Cl2 in doing this) and then, just replace the vessel w/the one w/H2SO4 & HgCl2 and add SCl2. Amazingly simple!
That is in theory, of course. In practice there's however une petite probleme - you can do it only in a fume cupboard. Controlling the temp should bee no problem, BUT - don't use anything other than glass all the way - SCl2 dissolves fucken anything (like rubber or PVC). Actually, when working w/small quantities, probably, some reactor similar to a test-tube could bee needed for better absorption of chlorine - so there might bee no alternative for hand-stirring the mixtr w/a thermometer during the addition, at least in SWIM's ghetto case. This would also mean an icebath can't bee used for cooling - at least, open icebath. Ice-cooled oilbath, maybee...
Ok, i realize i'm beginning to sound like FMAN now, just wanted to share my thoughts - maybee it helps.
SWIM personally has a neat self-made, albeit small, fume cupboard, which will probably do for him.
Um... It also occured to me now that both SCl2 and H2SO4 could bee cooled like to -25 C in a freezer prior to use, in which case it's not so one-pot no more, but definitely less hazardous than otherwise. BTW, they say - "not higher than 30 C", any ideas what it might mean? In SWIM's fucking experience, such mixtures (like an unstable/prone to oxidation compd. w/conc. H2SO4) are subject to various chain rxns, very exotermic :) :) :) - that is, if you hit 32 C, you may not only have some stuff evaporate, but it all may turn into an uncontrollable volcano, which will certainly make the place uninhabitable for a long time ;) Beware.
Antoncho