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ChemicalBook CAS DataBase List Tolclofos-methyl
57018-04-9

Tolclofos-methyl synthesis

2synthesis methods
-

Yield:-

Reaction Conditions:

with potassium carbonate in water;toluene

Steps:

1 EXAMPLE 1 (Compound No. 1):
EXAMPLE 1 (Compound No. 1): To a solution of 17.7 g. of 2,6-dichloro-4-methylphenol in 50 ml. of toluene was added 6.9 g. of potassium carbonate. Into the resulting mixture, 16.0 g. of O,O-dimethylthiophosphoryl chloride was dropped at 50° to 60° C. with stirring. After completion of the dropping, the stirring was further continued at 80° to 85° C. for 3 hours. Thereafter, the reaction liquid was cooled to 20° to 25° C. and then charged with water to separate the liquid into water and toluene layers. The toluene layer was dried with 5 g. of Glauber's salt. Subsequently, the Glauber's salt was separated by filtration, and the toluene was removed by distillation, whereby a solid residue was formed. This residue was recrystallized from methanol to obtain 20.3 g. of white crystals of O,O-dimethyl O-2,6-dichloro-4-methylphenyl phosphorothioate having a melting point of 79° to 79.5° C.

References:

Sumitomo Chemical Company, Limited US4039635, 1977, A

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