摘要:
The present invention provides a process of making 2-(methylthio)-5-(trifluoromethyl)-1,3,4-thiadiazole. The process includes the steps of (a) reacting methyldithiocarbazinate with a molar excess of trifluoroacetic acid; and (b) removing the water and excess trifluoroacetic acid. Water and excess trifluoroacetic acid are preferably removed via distillation.
摘要:
Disclosed herein is an improved process for preparing a thiophosphoryl chloride comprising reacting sulfur with a phosphorous trichloride, the improvement comprising a catalytic amount of a tertiary amine catalyst.
摘要:
The present invention provides a process for making sulfoxides from sulfides. The process includes the step of selectively oxidizing a sulfide utilizing a perborate or a percarbonate as an oxidizing agent.
摘要:
The present invention relates to an improved process for the preparation of thiophosphoryl chloride which is useful as an intermediate for the synthesis of insecticidally active compounds. The improvement comprises the presence in the reaction mixture of a catalytic amount of a nitroxide free radical of the following general formula: wherein R1, R2, R3 and R4 represent an alkyl group.
摘要:
The present invention provides a process for making 2-(methylthio)-5-(trifluoromethyl)-1,3,4-thiadiazole. The process includes the steps of reacting methyidithiocarbazinate with trifluoroacetic acid, in the absence of phosphorus trichloride, to form a mixture of 2-(methylthio)-5-(trifluoromethyl)-1,3,4-thiadiazole and 2,5-bis-(methylthio)-1,3,4-thiadiazole. Further, the process of the present invention includes selectively removing the 2,5-bis-(methylthio)-1,3,4-thiadiazole by acidifying the reaction mixture, and then separating the aqueous and organic phases.
摘要:
Disclosed herein is a process for preparing a phosphorodichloridodithioate comprising reacting a mercaptan, phosphorus trichloride, thiophosphoryl chloride and sulfur in the presence of a base catalyst.
摘要:
Disclosed herein is an aqueous process for preparing high yields of methyl dithiocarbazinate by reacting carbon disulfide and hydrazine in an effective ratio, in an aqueous medium to form hydrazinium dithiocarbazinate salt followed by methylating the hydrazinium dithiocarbazinate with methyl bromide.
摘要:
The invention is directed to a process for producing a stable, low odor S,S,S-tributylphosphorotrithioate having a level of dibutyl disulfide of 0.3% by weight or less. The process broadly includes the steps of a) reacting S,S,S-tributylphosphorotrithioite with an oxidizing agent to produce a crude S,S,S-tributylphosphorotrithioate, b) treating the crude product with sodium bisulfite to decompose any excess oxidizing agent, c) adding a caustic solution having a caustic concentration of from 25 to 50% by weight directly to the reaction mixture of step b), the addition of said caustic solution being stopped once the total caustic concentration is less than 10% by weight and once the pH is constant, and d) phase separating S,S,S-tributylphosphorotrithioate from the mixture of step c).
摘要:
Disclosed herein is a process for preparing a phosphorodichloridodithioate comprising reacting a mercaptan with a phosphorus trichloride and sulfur in the presence of an amine catalyst.
摘要:
Oxiranes are made from ketones by heating a ketone which is preferably an alkyl ketone to a temperature of from about 60.degree. to about 90.degree. C. (preferably about 80.degree. C.) in the presence of a sulfonium salt, a quaternary ammonium salt and a potassium hydroxide solution which is at least 61% potassium hydroxide. It is preferred that no organic solvent be included in the reaction mixture. The potassium hydroxide is generally included in an amount such that for every mole of ketone, from about 3 to about 4 moles of potassium hydroxide are present. The sulfonium salt is generally used in an amount of at least 1.1 moles for each mole of ketone. The quaternary ammonium salt is generally used in an amount of from about 1 to about 5 mol % based on moles of ketone present.