Does that first 3 i.e. --> 3Cl3P=NSO2Cl infront of the molecular
formula indicate the polymer form? or just a mistake? should be
infront of the brackets?
Without the 3 that formula corresponds to Trichlorophosphazosulfonyl chloride.
the monomer:
CAS 14700-21-1 Cl3P=N-SO2Cl
A synthesis of this is detailed in
Inorganic Chemistry, Vol. 18, No.4 1979.
Experimental:
Obviously this is a large scale synthesis and I do not take any
responsibility whatsoever of anyone repeating this experiment. The
source is from the above reference and should be conducted by a
professional in a professional laboratory. Carbon Tetrachloride is a
known carinogen, PCl5 and sulfamoyl chloride is corrosive and toxic.
Extreme care is advised when attempting this synthesis. Perhaps
scaling down 300 times might be an ideal starting point.
Trichlorophosphazosulfonyl Chloride.
To a 1-L, three-necked flask containing 200 mL of carbon tetrachloride
and equipped with an inlet tube, drying tube, and mechanical
stirrer was added 332 g (1.59 mol) of PCl5 through gooch
tubing. This was followed by 174 g (1.51 mol) of sulfamoyl chloride
added in the same manner. After stirring of the mixture for 1 h at
room temperature, the drying tube was replaced by a condenser and
the slush was refluxed for 2 h to give a clear yellow solution. After
removal of the solvent in vacuo, the residue crystallized on standing
in a refrigerator for 24 h. The solid was filtered in a drybox and
washed with 50 mL of cold n-heptane to give 250 g of product, mp
30-33 C. An additional 40 g (total yield 77%) was recovered from
the chilled filtrate. |
