Comments & criticisms please:
SWIM wasted her supply of SOCl2 in an incident that could have been prevented with a suck back trap. She wasn't that perturbed (she's become blase' about mishaps & near fatal gassings) until the chem supply house informed her that SOCl2 is now considered too hazardous for sale. That was troubling news, but since her philosophy is to use supply houses only for innocuous and unsuspicious chemicals anyhow, she decided to investigate the possibility of OTC SOCl2.
What she has come up with is this theoretical approach:
1. Cl2 + 2S = S2Cl2, according to US3992509
2. (a) S2Cl2 + Cl2 = SCl2 i.e. generated in situ
(b) 2H2SO4 + 3SCl2 + Cl2 = 2SOCL2 + 3SO2 + 4HCl
(catalyst = HgCl2), according to US1861900
Progress so far:
S2Cl2 was generated by passing dry Cl2 thru molten S (about 200 g initial charge) and condensing the exit vapor.
Don't have time to supply complete practical info (assuming anyone wants them I can produce later), but important notes I can think of now, are:
a. Temp must be fairly high (200 to 300 °C)
b. S must always be in excess. Fortunately it's cheap & OTC.
c. Cl2 generated by dripping 15% bleach into conc. HCl. Can't remember quantities right now. This method superior to HCl + KMnO4.
d. Cl2 bubbled thru S. Temps high enough so that plugging of gas dispersion tube not a problem.
e. Small amount (< 1/2 g) of 'Ferric chloride' used as a catalyst. 'Ferric chloride' made by leaving 3 or 4 nails in a few ml conc. HCl overnight, filtering ppte and drying in oven.
f. No absorbtion device for unreacted Cl2 was used. Fortunately it seemed that just about all the CL2 reacted.(By now SWIM swears she's immune to the stuff anyhow).
g. About 80 ml (~ 120 g) of ye old amber liquid with an unpleasant odor was produced. Not sure about purity. However very little S floating around. Also contamination with SCl2 will not be a problem since the idea is to generate it in rctn 2(a) anyway. Therefore it has not been distilled and currently sits in a fridge. Do hope it doesn't react to polysulfides (see
Post 208279
(Antoncho: "Re: An easy OTC 2,5-diMeO-phenylmercaptan", Novel Discourse)).
Overall procedure is similar to
Post 208025
(Antoncho: "Preparation of S2Cl2", Novel Discourse) &
Post 208077
(catastrophe: "Re: Preparation of S2Cl2", Novel Discourse) just at higher temps.
Questions for the bees:
1. How to clean a pile of sulfur fouled glassware (SWIM got no CS2) ?
2. Ultimately SOCL2 could be used for 3,4,5-TMB-COOH + SOCL2 = 3,4,5-TMB-COCl. Any ideas on using S2Cl2 itself for this reaction ? In
Post 229993
(foxy2: "Acetyl Chloride/Acid chloride production!", Chemistry Discourse) some patents were described for methyl substituted aromatic acid chlorides but nothing on methoxy versions.
Oh one last point of clarity:
SOCL2 = Thionyl Chloride
SO2CL2 = Sulfuryl Chloride
S2Cl2 = Disulfur dichloride, often called 'Sulfur monchloride'
SCl2= Sulfur dichloride
,just in case there is still confusion.