4637-24-5Relevant articles and documents
Method for synthesizing 2-amino-5-nitrothiazole
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Paragraph 0037-0039; 0043-0050, (2020/08/06)
The invention discloses a method for synthesizing 2-amino-5-nitrothiazole, which comprises the following steps: (1) in an inert atmosphere, adding diethylamine, acetyl chloride and triethyl orthoacetate into a reaction container, uniformly mixing, stirring to react for 12-24 hours, and distilling and purifying the reaction product to obtain N, N-dimethylformamide dimethyl acetal, (2) in an inert atmosphere, mixing N, N-dimethylformamide dimethyl acetal with nitromethane, heating the mixture to 80-100 DEG C for reflux reaction, carrying out reduced pressure distillation on the reaction productto remove the solvent, and purifying to obtain N, N-dimethyl nitroethylene, and (3) in an inert atmosphere, putting N, N-dimethyl nitroethylene into a reaction container, sequentially adding ethanol,liquid bromine and thiourea, reacting at room temperature, after the reaction is finished, filtering a reactant, washing with ice ethanol, drying to obtain a white solid, adding water, and filtering to obtain the 2-amino-5-nitrothiazole. According to the method for synthesizing 2-amino-5-nitrothiazole, the raw materials are easy to obtain, the cost is low, and the yield can reach 60%.
Preparation method of azoxystrobin intermediate
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Paragraph 0036; 0037; 0038, (2018/09/29)
The invention relates to a preparation method of an azoxystrobin intermediate. According to the method, a compound shown in a formula (II) serves as a raw material and reacts with a methylating agentunder a basic condition to obtain the azoxystrobin intermediate shown in a formula (I), wherein Z1 represents halogen. The method has the advantages that the reaction time is short, the total yield ishigh, the cost of raw materials is low, and the method is suitable for large-scale production and has very important significance for industrial production of final products of azoxystrobin. The formula (II) and the formula (I) are shown in the description.
N,N-dimethylformamide dimethyl acetal synthesis method
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Paragraph 0034-0037; 0048-0049, (2017/06/13)
The invention discloses an N,N-dimethylformamide dimethyl acetal synthesis method. The synthesis method includes: subjecting N,N-dimethylformamide and dimethyl sulfate to reaction to generate an imine complex, and subjecting the imine complex and solid sodium methylate dispersed in an organic solvent to reaction to obtain N,N-dimethylformamide dimethyl acetal, wherein the organic solvent refers to at least one of isoparaffin, solvent oil and white oil. By adoption of the novel organic solvent, reaction conditions (with the temperature being 20-30DEG C) of the imine complex and the sodium methylate can be lowered, and the reaction conditions are milder. In addition, when the reaction temperature is compared with an original reaction temperature ranging from -5 DEG C to 0 DEG C, products generated after reaction are quicker in dissolution and can be timely dissolved in the organic solvent to be wrapped by the organic solvent, so that by-product generation is avoided, and yield is increased. According to experiments, yield of the N,N-dimethylformamide dimethyl acetal can reach 85% above.