- Synthesis method of N-hydroxymethyl-3, 4, 5, 6-tetrahydrophthalimide
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The invention discloses a synthesis method of N-hydroxymethyl-3, 4, 5, 6-tetrahydrophthalimide, which comprises the following steps of adding phthalimide and tetrabutylammonium bromide into water, dropwise adding a formaldehyde aqueous solution after adding, carrying out heat preservation reaction after dropwise adding, drying a solvent after reaction, recrystallizing by using an acetone aqueous solution, putting the recrystallized material into a high-pressure kettle, adding Pd/C, introducing hydrogen, conducting heat preservation and pressure retaining reaction, desiccating the solvent and recrystallizing toluene after the reaction is finished. According to the method, the two-step synthesis yield of the method can reach 80% or above, and the normalized content of a product liquid spectrum can reach 97.6%. The solvent used in the method can be used in a reaction system after being recycled, the reduction catalyst can be used for more than 10 times, and the method is simple in process, easy to operate, high in reaction selectivity, low in product yield, quality and energy consumption and free of phosphorus and nitrogen-containing wastewater, the production field environment is remarkably improved, and industrial clean production is facilitated.
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Paragraph 0010; 0030-0031; 0036-0041; 0046-0049
(2021/06/13)
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- Preparation method of N-hydroxymethyl-3,4,5,6-tetrahydroimine
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The invention relates to a preparation method of N-hydroxymethyl-3,4,5,6-tetrahydroimine, which comprises the following steps: by using 3,4,5,6-tetrahydrophthalimide as a raw material, adding a formaldehyde solution and a potassium carbonate solution, regulating the pH value, carrying out reflux reaction, removing wastewater, removing the solvent under reduced pressure, performing cooling crystallization, and drying to obtain a white solid, N-hydroxymethyl-3,4,5,6-tetrahydroimine. The preparation method disclosed by the invention has the beneficial effects that good reaction conditions are obtained by using a special solvent and a specific feeding sequence at a specific temperature, the reaction is mild and controllable, the solvent recovery rate is high, and the product yield is high; inaddition, a mother liquor product is subjected to secondary reaction, equipment investment is reduced, and the production period is shortened.
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Paragraph 0024-0035
(2020/11/22)
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- Process for producing cyclopropanecarboxylates
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There is disclosed a process process for producing a cyclopropanecarboxylate of formula (1): 1which process comprises reacting cyclopropanecarboxylic acid of formula (2): 2with a monohydroxy compound of formula (3): R6OH??(3),in the presence of a catalyst compound comprising an element of to Group 4 of the Periodic Table of Elements.
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