593-56-6Relevant articles and documents
Preparation method O - alkyl substituted hydroxylamine salt
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Paragraph 0078-0081, (2021/11/14)
The invention relates to a preparation method of N - alkyl substituted hydroxylamine salt, and belongs to fine chemical engineering. Pesticide or bulk pharmaceutical chemicals technical field. The present invention reacts with the N - alkyl of the oxime with an inorganic salt of hydroxylamine to give N - alkyl-substituted hydroxylamine salt and oxime. The invention provides an efficient and environment-friendly method for preparing N - alkyl substituted hydroxylamine salt, and simultaneously, an N - alkyl substituted hydroxylamine salt is prepared, and the oxime can be re-prepared to form N - alkylate of oxime so as to realize the material circulation. No equivalent acid is used in the reaction process. Alkali neutralization, avoided the current method to use a large amount of acid, alkali and produce inorganic salt solid waste shortcoming, environmental protection more. The preparation method is mild in reaction condition, and the defects of high pollution and high energy consumption of the traditional process are overcome. In-flight R1 , R2 What is R is as claimed in the claims and the description.
Preparation method of methoxyamine hydrochloride and preparation method of N-methoxyacetamide
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Paragraph 0038-0052, (2021/05/29)
The invention relates to a preparation method of methoxyamine hydrochloride and a preparation method of N-methoxyacetamide, belonging to the technical field of organic synthesis. The preparation method of the methoxyamine hydrochloride comprises the following steps: 1) carrying out a methylation reaction on acetohydroxamic acid and dimethyl sulfate in water to generate N-methoxyacetamide, wherein in the process of the methylation reaction, sodium bicarbonate and sodium hydrogen salt are adopted to control the pH value of a reaction system to be 7-9, and a molar ratio of sodium bicarbonate to sodium hydroxide is (0.03-0.09): 1; and 2) preparing methoxyamine hydrochloride from N-methoxyacetamide. According to the preparation method of methoxyamine hydrochloride, composite alkali of sodium bicarbonate and sodium hydroxide is adopted in the methylation reaction process, so the conversion rate of acetohydroxamic acid can be increased, the pH value in the methylation process can be strictly controlled to be 7-9, generation of polymethylation impurities (O,N-dimethylhydroxylamine hydrochloride) is reduced, and the yield of N-methoxyacetamide is improved.
Palladium-catalyzed regio- And stereoselective access to allyl ureas/carbamates: Facile synthesis of imidazolidinones and oxazepinones
Banerjee, Prabal,Saha, Debarshi,Taily, Irshad Maajid
supporting information, p. 6564 - 6570 (2020/11/10)
Typically, transition metal catalysis enforces the stereodefined outcome of a reaction. Here we disclose the palladium-catalyzed regio- and stereoselective access to allylic ureas/carbamates and their further exploitation to diverse cyclic structures under operationally simple reaction conditions. This protocol features palladium-catalyzed decarboxylative amidation of highly modular VECs with good to excellent yield, minimal waste production, wide substrate scope, and low catalyst loading. In follow-up chemistry, we demonstrated the debenzylation of vinylic imidazolidinones to N-hydroxycyclic ureas and regioselective derivatization towards the facile synthesis of halohydrins and oxiranes under mild reaction conditions in good to excellent yields. This journal is