Patent GB-774276-A (GB)
Title: Manufacture of the compounds concis, concis and concis
IPC: C01B21/083
Filed: 1953-03-24
Abstract: One or more of the compounds CO3NCIS, CO6NCIS2 and C2O3N2Cl2S are obtained by reacting cyanogen chloride and sulphur trioxide.  The sulphur trioxide may be solid, liquid, or gas, mixtures of gas with an inert gas, or mixtures of liquid sulphur trioxide and sulphur dioxide.  The cyanogen chloride may be solid, liquid or gas depending on the temperature.  CO6NClS2 and C2O3N2Cl2S are produced preferentially when liquid sulphur trioxide is run while stirring and cooling into cyanogen chloride at low temperature preferably 0 to - 30 DEG  C.  The liquid compound CO6NClS2, which is the main product, is isolated by distillation under reduced pressure, and a crystalline precipitate of C2O3N2Cl2S can be isolated by filtering with suction before distillation or remains in the residue after distillation. Some CO3NClS is formed in the low temperature reaction and an example (2) indicates the method of separating the three compounds. CO3NClS may also be formed preferentially by reacting sulphur trioxide and cyanogen chloride in the molar ratio 1 : 1 at above 100 DEG  C., preferably 130-150 DEG  C., by decomposition of CO6NClS2 at atmospheric pressure, by reacting CO6NClS2 with cyanogen chloride in the molar ratio 1 : 1 at above 100 DEG  C., preferably 120-140 DEG C., by reacting CO6NClS2 and C2O3N2Cl2S in equimolar proportions at above 100 DEG  C., preferably 120-150 DEG  C., or by reacting cyanogen chloride at above 100 DEG  C. preferably 130-140 DEG  C. with the crude reaction product of sulphur trioxide and cyanogen chloride at low temperature which contains mainly CO6NClS2 and C2O3N2Cl2S.  The reactions are usually effected at atmospheric pressure but CO3NClS may be prepared by reacting sulphur trioxide and cyanogen chloride at superatmospheric pressure.  The reactants may be in solution, e.g. in cyanogen chloride or sulphur dioxide and in this way C2O3N2Cl2S is formed preferentially.  The formul  of the compounds are stated to be O = C = N-SO2Cl, O = C = N-SO2-O-SO2Cl and: <FORM:0774276/IV(b)/1>ALSO:One or more of the compounds CO3NClS, CO6 N Cl S2 and C2 O3 N2 Cl2 S are obtained by reacting cyanogen chloride and sulphur trioxide.  The sulphur trioxide may be solid, liquid, or gas, mixtures of gas with an inert gas, or mixtures of liquid sulphur trioxide and sulphur dioxide.  The cyanogen chloride may be solid, liquid or gas depending on the temperature.  CO6 N Cl S2 and C2 O3 N2 Cl2 S are produced preferentially when liquid sulphur trioxide is run while stirring and cooling into cyanogen chloride at low temperature preferably 0 to -30 DEG C. The liquid compound CO6 N Cl S2, which is the main product, is isolated by distillation under reduced pressure, and a crystalline precipitate of C2 O3 N2 Cl2 S can be isolated by filterin with suction before distillation or remains in the residue after distillation.  Some CO3 N Cl S is formed in the low temperature reaction and an example (2) indicates the method of separating the three compounds. CO3 N Cl S may also be formed preferentially by reacting sulphur trioxide and cyanogen chloride in the molar ratio 1:1 at above 100 DEG C., preferably 130-150 DEG C., by decomposition of CO6 N Cl S2 at atmospheric pressure, by reacting CO6 N Cl S2 with cyanogen chloride in the molar ratio 1:1 at above 100 DEG C., preferably 120-140 DEG C., by reacting CO6 N Cl S2 and C2 O3 N2 Cl2 S in equimolar proportions at above 100 DEG C., preferably 120-150 DEG C., or by reacting cyanogen chloride at above 100 DEG C. preferably 130-140 DEG C. with the crude reaction product of sulphur trioxide and cyanogen chloride at low temperature which contains mainly CO6 N Cl S2 and C2 O3 N2 Cl2 S.  The reactions are usually effected at atmospheric pressure but CO3 N Cl S may be prepared by reacting sulphur trioxide and cyanogen chloride at super-atmospheric pressure.  The reactants may be in solution, e.g. in cyanogen chloride or sulphur dioxide and in this way C2 O3N2 Cl2 S is formed preferentially. The formul  of the compounds are stated to be O=C=N-SO2 Cl, O=C=N-SO2-O-SO2 Cl and <FORM:0774276/III/1>