74222-95-0Relevant articles and documents
Production process for improving quality of sulfonyl isocyanate
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Paragraph 0025-0030, (2021/03/30)
The invention discloses a production process for improving the quality of sulfonyl isocyanate. The production process comprises the steps of mixing a sulfanilamide raw material and xylene according toa certain ratio to form a sulfanilamide solution, adding a certain amount of xylene into a synthesis kettle, heating, controlling the temperature at 110 to 115 DEG C, adding the sulfanilamide solution into the synthesis kettle through a transfer pump at a certain rate; dropwise adding a catalyst and introducing gaseous phosgene at the same time, paying attention to that the catalyst must be dropwise added 2 hours before the sulfanilamide solution is well converted, reducing the phosgene flow until the process requirement cumulant is reached, transferring a product into a light breaking kettleafter heat preservation is performed for 2 hours, removing redundant phosgene by using nitrogen, and finally obtaining a finished product after qualified sampling and analyzing. According to the invention, the synthesis system of sulfonyl isocyanate is optimized, the yield of sulfonyl isocyanate is improved, and meanwhile, the synthesized tail gas and the gas-driving tail gas are innovatively condensed by a condenser and then flow back to the synthesis kettle, so that the tail gas is recycled, and the reaction rate and content of the product are improved.
Synthetic process of metsulfuron-methyl-D3
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Paragraph 0049-0051, (2019/10/07)
The invention provides a synthesis process of metsulfuron-methyl-D3, comprising the following steps: Step 1), adding a compound I in an ethanol solution of sodium ethoxide to prepare a compound II; Step 2), adding the compound II prepared in the Step 1) into a tetrahydrofuran solution of deuterated sodium methoxide, and refluxing to obtain a compound III; Step 3), suspending a compound IV in anhydrous toluene, dropwise adding a compound V, adding triethylene diamine, and heating to prepare a toluene solution of a compound VI; and Step 4), suspending the compound III prepared in the Step 2) in ethyl acetate in under nitrogen protection, heating and dropwise adding the toluene solution of the compound VI that is obtained in the Step 3), and reacting to prepare the final product metsulfuron-methyl-D3. The invention has the following technical effects: by conversion of the functional group of a relatively-cheap compound I, the compound III is synthesized; although the yield is low, cumbersome multi-step synthesis and the use of a large amount of expensive deuterated methanol are avoided.
Collection of ion-trap mass spectre of sulfonylurea pyrolysis products
Galletti,Dinelli,Chiavari
, p. 333 - 338 (2007/10/02)
The pyrograms of 14 sulfonylureas, i.e. herbicides characterized by high biological activity and low application dose are discussed and the mass spectra of over 30 relevant pyrolysis products as obtained with a heated filament pyrolyzer interfaced to a capillary gas chromatograph/ion-trap detector mass spectrometer are presented. Such a data compilation is useful for diagnostic purposes for both intact sulfonylureas and their metabolites after degradation in soil, because metabolites and pyrolysis products are often identical and most of their mass spectra are lacking in commercially available mass spectral libraries. The performance of the ion-trap detector based on the quality of the mass spectra is briefly discussed.
