10-31-03 20:48
No 468059
Another similar synthesis, generating sulfur chloride in situ:
Mix quickly and thoroughly 205-215 g of pulverized fine NaOAc and 10g dry sulfur powder, the mixture is quickly transferred to a wide-mouth 1 liter RBF and wetted w/25 ml acetic anhydride. Into the flask through the rubber cork extend 1) a wide tube for chlorine in-flow 2) an overhead stirrer, which is sealed with the aid of a piece of rubber tubing greased with vaseline and 3) an out-leading tube for excess Cl2 release. The flask is immersed in an ice-bath. Chlorine is initially passed in very carefully, with frequent stirring or shaking, over the passage of time the rxn gets hotter and more and more liquid, so the stirrer may bee after some time rotated with a motor. Chlorine stream should bee regulated so that almost all of it is absorbed. When the reaction mixture stops heating and Cl2 is no longer taken up, the rxn contents are distilled in vacuo at oil bath temp ~150-180°C, then redistilled at ordinary pressure, collecting the fraction boiling between 132 and 142°C. Yield ~90%.
Has anyone tried this without using the AA as a pre-wetting agent, Would it work ok, the first time around, but with a lower yield?, say if you substituted GAA instead,.
Sure would be nice.!
hm
"back in my day,..we used to call them tubes, Girls that is..."
(Newbee)
11-03-03 10:33
No 468507
As i understood u need it to prepare the Acidchlorides to synth the Aceticanhydrid right ?
Ok this is a very unusual way but i hope i can help u a bit.
U will need SOCl2 to prepare the Acidhalogenides. This will be couterproductive because u will need PCl5 to prepare SOCl2.
PCl5 + SO2 --> SOCl2
SO2 + Cl2 --> SO2Cl2
S + Cl2 --> S2Cl2
These reaktions can only be made under very dry conditions as the products are very moisture sensitive.
Economical i would prefer the route via PCl3 to yield the Acidchlorides.
The preparation "in situ" isnt possible because many byproducts will form and ull have to purify ur product first. Another problem ist the cost of these raktions....time is money...
But if u wanna experiment a bit just try this :
penetrate CH3COOH in waterfree, but protic solvent by Cl2.
Perhaps some CH3COCl will form and u can distill it ???
(Newbee)
11-03-03 10:51
No 468511
Here s the preparation of Disulfurdichlorid:
In a little keramik ship Sulfur is dried in an explosion-tube. Dry 2 or 3 times by vakuum/argon. Fit a konz.H2SO4-gas-washing-bottle to the tube and at the other end a cooler to kondense the products. Let gas Cl2 trough the H2SO4 into the tube while gently heating the Sulfur. The Product will condense as a yellow or orange liquid wich is very, very stinky and smells so ugly that u will "run forest". Ok The color comes from byproducts like SCl2. destilll at ambient pressure at 137-138°C ur product will come over.
This is not a "kitchen reaktion"
Dont try this at home!
(that sounds crazy but when "i" say dont try this at home, ull better dont try this at home)
