C - Chemistry – Metallurgy – 07 – F
Patent
C - Chemistry, Metallurgy
07
F
260/537.7
C07F 9/34 (2006.01) C07F 9/42 (2006.01)
Patent
CA 1110274
IMPROVED PROCESS FOR PREPARING ALKYL OR ARYL THIOPHOSPHORUS HALIDES AND MIXED ISOMERS THEREOF Abstract Improved yields and a lower accumulation of by-product is obtained in the method for preparing compounds of the formula: Image wherein R is a C1 to C20 alkyl radical, cycloalkyl of 5-6 carbon atoms in the ring and the C1-C4 alkyl substituted deriva- tive thereof, an aralkyl radical of up to two fused rings, the alkyl portion having from 1 to 20 carbon atoms, an aryl radical of up to three fused rings and the C1-C4 alkyl derivatives thereof, and biphenyl and the C1-C4 alkyl derivatives thereof, X is a halogen of chlorine or bromine, and Z is either R or X, by the reaction of a phosphorus halide source, a hydrocarbon source selected from the group consisting of RH, RX and RSaR, wherein a is 1 or 2 and a sulfur source under autogenous pressure in an autoclave at a temperature ranging from about 175°C. to about 450°C. by recycling to successive runs a by-product of the reaction remaining after separation of the RP(S)XZ product fraction selected from the group con- sisting of: a) a by-product fraction having a boiling point lower than the product fraction; b) a by-product fraction having a boiling point higher than the product fraction; c) a by-product fraction having a boiling point higher than the product RP(S)XZ wherein Z is R fraction; d) XZP(S)RP(S)XZ e) liquid residue; f) solid residue; g) mixtures thereof; and h) mixtures of the preceding with R2P(S)X wherein R and X are as defined hereinbefore.
294847
Uhing Eugene H.
Via Francis A.
Gowling Lafleur Henderson Llp
Stauffer Chemical Company
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