- PROCESS FOR PREPARATION OF THIOPHOSPHORYL CHLORIDE AND ACEPHATE
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The present invention discloses an improved process for preparation of acephate and intermediates thereof. More particularly, the present invention relates to a process for preparation of thiophosphoryl chloride useful for commercial production of pesticides and pharmaceutically active compounds.
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Page/Page column 25
(2021/04/23)
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- Preparation method of insecticide acephate
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The invention discloses a preparation method of an insecticide acephate. The preparation method of the insecticide acephate comprises the steps that phosgene and O,O,O-trimethyl sulfydryl phosphate react under the action of a catalyst for 1-4 hours, excessive phosgene is removed through nitrogen purging after the reaction, vacuum distillation is performed to remove methylclhlorofonmate, and the obtained liquid is O,S-dimethyl phosphoryl chloride; acetamide is dropwise added to the toluene solution of the O,S-dimethyl phosphoryl chloride, then an acid-binding agent is added, heating is performed to reach 20-60 DEG C, stirring reaction is performed for 2-6 hours, cooling is performed to reach room temperature, mixed liquid is obtained, and the acephate is obtained through post-treatment. The reaction process of the insecticide acephate prepared by adopting the preparation method is simple, the conditions are mild, the reagent and energy consumption is reduced, the post-treatment process is simple, extraction is not needed, the final product can be obtained through simple filtration and crystallization, the problem of environmental polluting waste liquid and waste gas emissions is basically not produced, and the requirements of environmental protection and energy saving are met.
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Paragraph 0056; 0057; 0058
(2017/01/17)
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- A heterogeneous reaction
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The invention discloses a highly selective novel reaction with an important application value in organic phosphorus synthesis methodology. The reaction can be applied in important pesticide commodities of acephate, glyphosate, glufosinate-ammonium, chloramine phosphorus, profenofos, and the like. With the reaction, innovative technical synthetic routes can be designed. With the reaction, standards of clean production technologies can be satisfied, and the production cost is greatly reduced compared to existing technical routes.
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Paragraph 0125; 0126
(2017/02/24)
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- An insecticide acephate method for the continuous production of the
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The invention provides a continuous production method of acephate. The continuous production method comprises the following steps: (1) acylation reaction: continuously adding methamidophos, acetic anhydride, a solvent and a catalyst into an acylation device in a certain proportion, and reacting for 65-240 minutes at 20-80 DEG C to obtain a reaction liquid; (2) neutralization reaction: introducing the reaction liquid obtained in the step (1) into a neutralization reactor, and continuously mixing with ammonia or ammonia water for 5-60 minutes at 10-50 DEG C to obtain a neutralization liquid; (3) extraction: introducing the neutralization liquid into an extraction tower to perform reverse extraction; (4) evaporation and concentration: performing evaporation and concentration on an extraction liquid in a double-effect evaporator; and (5) crystallization and drying: crystallizing a concentrated extraction liquid at 5-25 DEG C, then filtering crystallized solids by virtue of a filtering machine, and finally drying the solids in a dryer to obtain acephate. The continuous production method provided by the invention achieves the continuous operation and automatic control in a production process of acephate, and has very strong practicability.
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Paragraph 0030; 0031; 0032
(2017/06/29)
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- Synthesis and characterization of O,S-dimethylphosphoramidothioate and N-acetyl O,S-dimethylphosphoramidothioate
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O,S-Dimethylphosphoramidothioate (methamidophos) and N-acetyl O,S-dimethylphos- phoramidothioate (acephate) were synthesized by new methods to investigate the structure-activity study of acetyl cholinesterase (AChE) inhibition through the parameters of logP,δ 31P, and IC 50. After their characterization by NMR (31P, 31P{1H}, 13C, and 1H), IR, and mass spectroscopy, logP and δ31P (31P chemical shift in NMR) were used to evaluate lipophilicity and electronical properties. The logP values for methamidophos and acephate were experimentally determined by the GC-shake-flask method, and the ability of the compounds to inhibit human AChE was evaluated by a modified Ellman's assay. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.
- Ghadimi,Mousavi,Rahnama,Rahimi
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scheme or table
p. 347 - 354
(2010/07/03)
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- Process for dry granulation by agitative balling for the preparation of chemically stable, dry-flow, low compact, dust free, soluble spherical granules of phosphoroamidothioate
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Chemically stable, dry-flow, low compact, dust free, soluble granules of phosphoroamidothioate are prepared using a substantially dry granulation process including an agitative balling process. In a preferred embodiment, spherically shaped acephate granules are produces without the intentional addition of water and/or solvents.
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- THIAZOLYL-SUBSTITUTED CARBOCYCLIC 1,3-DIONES AS PESTICIDAL AGENTS
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2-Azolyl-cycloalkane-1,3-dione derivatives (I) are new. 2-Azolyl-cycloalkane-1,3-dione derivatives of formula (I), are new: Het = 5-membered nitrogen-containing heterocycle (optionally substituted (os) by halo, (halo)alkyl, (halo)alkoxy, (halo)alkenyloxy, CN, NO2, alkylthio, alkylsulfinyl, alkylsulfonyl, os phenyl or phenoxy), preferably triazolyl; m = 0 or 1; A = H; alkyl, alkenyl, (poly)alkoxyalkyl or alkylthioalkyl (all os by halo); os unsaturated cycloalkyl (in which at least one ring atom is optionally replaced by a heteroatom); or (hetero)aryl or aralkyl (all os by halo, (halo)alkyl, (halo)alkoxy, CN or NO2); A' = H or alkyl; or CAA' = os ring (in which at least one ring atom is optionally replaced by a heteroatom); or A + Q1 = os alkanediyl, in which two non-adjacent C-atoms may together form a further os ring; Q1 = H, (alkoxy)alkyl, os cycloalkyl (in which a ring CH2 is optionally replaced by O or S); or phenyl(alkyl) or heteroaryl(alkyl) (all os); Q2 - Q4 = H or alkyl; or CQ1Q2 = CAA'; G = H, -COR1, -C(L)-MR2, -SO2R3, -P(L)R4R5, E or -C(L)-NR6R7; E = metal or ammonium ion; L, M = O or S; R1 = alkyl(thioalkyl), alkenyl, alkoxyalkyl or polyalkoxyalkyl (all os by halo); cycloalkyl (os by halo, alkyl or alkoxy, and optionally interrupted by at least one heteroatom); or phenyl(alkyl), phenoxyalkyl or heteroaryl(oxyalkyl) (all os); R2 = (alkoxy)alkyl, alkenyl or polyalkoxyalkyl (all os by halo); or cycloalkyl, phenyl or benzyl (all os); R3 = (halo)alkyl, phenyl or benzyl (all os); R4, R5 = alkyl, alkoxy, mono- or dialkylamino, alkylthio, alkenylthio or cycloalkyl (all os by halo); or phenyl, benzyl, phenoxy or phenylthio (all os); and R6, R7 = H; (cyclo)alkyl, alkenyl or alkoxy(alkyl) (all os by halo); or phenyl or benzyl (both os); or NR6R7 = heterocycle (optionally interrupted by O or S). An Independent claim is also included for the preparation of (I).
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Page/Page column 56
(2008/06/13)
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- Method for purifying O,S-dimethyl N-acetylphosphoramidothioate
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A method for purifying O,S-dimethyl N-acetyphosphoramidothioate, which is characterized by subjecting a crude crystal of O,S-dimethyl N-acetylphosphoramidothioate to recrystallization by using a two-phase solvent system comprising water and an organic which is an aromatic hydrocarbon, an aliphatic carboxylic acid ester or aliphatic ketone, wherein the amount of water is 0.1 to 2 parts by weight and the amount of the organic solvent is 1 to 20 parts by weight to 1 part by weight of the crude O,S-dimethyl N-acetylphosphoramidothioate. A further method for purifying O,S-dimethyl N-acetylphosphoramidothioate, which is characterized by extracting O,S-dimethyl N-acetylphosphoramidothioate from an aqueous solution of crude O,S-dimethyl N-acetylphosphoramidothioate with an organic solvent which is a carbonate ester, an aliphatic carboxylic acid ester, an aliphatic ketone, an aliphatic alcohol or a mixture of two or more thereof, wherein the solubility of water in the organic solvent is in a range of from 1 to 20% by weight, and crystallizing O,S-dimethyl N-acetylphosphoramidothioate from the resulting organic phase.
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- Macrocyclic plant acaricides
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Compounds of the formula I STR1 in which either R is methyl and there is a double bond in the 9,10-position, or in which R is hydrogen and there is a single bond in the 9,10-position, are highly active against Acarina which damage plants.
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- Nitro- and cyanoguanidines as selective preemergence herbicides and plant defoliants
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There are provided novel nitroguanidine and cyanoguanidine compounds. A method of dessicating and defoliating plants by applying to the foliage thereof certain nitroguanidine or cyanoguanidine compounds and a method for the selective preemergence control of undesirable broadleaf weeds and grasses in the presence of graminaceous crops are disclosed.
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- Divalent metal salts of O,S-dialkyl-N-alkanoylphosphoroamidothioates
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Calcium and barium bis-O,S-dialkyl-N-alkanoylphosphoroamidothioate salts have high insecticidal activity and are substantially more stable than the corresponding O,S-dialkyl-N-alkanoylphosphoroamidothioate compound.
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