- Synthesis method of O-formate benzyl sulfonamide
-
The invention discloses a synthesis method of ortho-formate benzyl sulfonamide, and relates to the technical field of battery electrolyte additives. The method comprises the following steps: taking 2 - chloromethyl benzoate as a raw material, and performing nucleophilic substitution reaction. The oxidation chlorination reaction, the ammoniation reaction and the tert-butyl protection are obtained, that is, the ortho-formate benzyl sulfonamide. To the invention, a plurality of reaction kettles are used for gradually synthesizing the ortho-formate benzyl sulfonamide, the direct connection relation between each product is isolated, the influence of byproducts generated by the solvent on different reactions is avoided, and the purity of the product is further improved by adopting a method of distilled water washing, ethyl acetate extraction and anhydrous magnesium sulfate drying. The total yield of the synthesis method reaches above 59.96%, and the purity of the ortho-formate benzyl sulfonamide reaches 99.5% or above.
- -
-
-
- Production method of methyl o-formate benzyl sulfonamide
-
The invention belongs to the technical field of pesticide intermediates, and particularly relates to a production method of methyl o-formate benzyl sulfonamide. The production method comprises steps:reacting o-methylbenzoic acid with sulfuryl chloride to obtain o-chloromethylbenzoic acid; reacting o-chloromethylbenzoic acid with methanol to obtain o-chloromethyl methyl benzoate; reacting o-chloromethyl methyl benzoate with sodium thiosulfate to obtain methyl o-formate benzyl mercaptan, reacting methyl o-formate benzyl mercaptan with chlorine to obtain methyl o-formate benzyl sulfonyl chloride, and reacting methyl o-formate benzyl sulfonyl chloride with ammonia gas to obtain methyl o-formate benzyl sulfonamide. According to the method, polychlorinated side reactions in the production process are reduced, the yield is increased, the tar yield is reduced, and the problems of low yield and high cost in the production process are solved.
- -
-
Page/Page column 6-9
(2020/09/12)
-
- Development of an immunoassay for the residues of the herbicide bensulfuron-methyl.
-
To develop a competitive indirect enzyme-linked immunosorbent assay based on polyclonal antibodies for the detection of the sulfonylurea herbicide bensulfuron-methyl, seven structurally related haptens were synthesized. Four of them mimicking the target analyte were conjugated to keyhole limpet hemocyanin by the N-hydroxysuccinimide activated ester method to use as immunogens, and all of them were conjugated to bovine serum albumin to use as plate-coating antigens. Polyclonal antibodies raised in rabbits and the coating antigens were screened and selected for the assay in simple homologous and heterologous ELISA formats. Three sensitive heterologous ELISAs were selected and optimized, showing the average IC(50) values of bensulfuron-methyl as low as 0.17, 0.09, and 0.09 ng/mL, the detection ranges of 0.04-0.60, 0.01-0.60, and 0.04-0.25 ng/mL, and the lowest detection limits of 0.03, 0.002, and 0.03 ng/mL, respectively. The cross-reactivities of other sulfonylurea herbicides and metabolites of bensulfuron-methyl to the antibodies were less than 15% in the two assays. Recoveries from the analyte-fortified water samples in assay I were in the range of 81-125% by simple dilution. The correlation between the ELISA and HPLC was 0.999 (n = 15) with a slope of 1.37 in the analysis of groundwater samples fortified with bensulfuron-methyl. The results obtained strongly indicate that the ELISA can be a highly sensitive and convenient tool for detecting bensulfuron-methyl residues in agricultural and environmental samples.
- Lee, Jae Koo,Ahn, Ki Chang,Park, Oee Sook,Ko, Yong Kwan,Kim, Dae-Whang
-
p. 1791 - 1803
(2007/10/03)
-
- Herbicidal compounds, their production and use
-
A compound of the general formula STR1 wherein R1 is a phenyl group which may be substituted, R2 and R3 respectively are a lower alkyl or lower alkoxy group, Z is CH or N and n is 0 or 1, or a salt thereof which is useful as a herbicide.
- -
-
-