41317-15-1Relevant articles and documents
Synthesis of 2-methyl-4-methoxydiphenylamine by palladium catalyzed C-N coupling - High synthetic versatility by use of a flexible catalytic system
Scholz, Ulrich,Schlummer, Bj?rn
, p. 6379 - 6385 (2005)
The synthetic versatility of the Buchwald-Hartwig Amination is demonstrated by the synthesis of the industrially important intermediate 2-methyl-4-methoxydiphenylamine. Using four routes differing in the choice of the starting materials, the diarylamine could be synthesized in excellent yields, however, each reaction required a different combination of ligand, base and solvent. This new approach is compared to established industrial routes.
Preparation method and application of 2-methyl-4-methoxydiphenylamine
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Paragraph 0070-0098, (2021/06/23)
The invention relates to the field of preparation of diphenylamine, in particular to a preparation method and application of 2-methyl-4-methoxydiphenylamine, and the preparation method of the 2-methyl-4-methoxydiphenylamine comprises the following steps: (1) in a solvent, reacting 2-methyl-4-methoxyaniline with halogenated benzoic acid in the presence of a catalyst and an acid-binding agent to obtain a condensation product, wherein the acid-binding agent is selected from one or more of carbonate, phosphate and hydroxide of alkali metal; (2) acidifying the condensation product, and conducting filtering, washing and drying to obtain a product 1; and (3) decarboxylating the product 1, and conducting purifying to obtain the product 1. The preparation method of the 2-methyl-4-methoxydiphenylamine is convenient to operate, short in time and suitable for large-scale production, and the production efficiency is greatly improved.
Synthesis method of DPA
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Paragraph 0007, (2020/01/25)
The invention discloses a synthesis method of DPA. The method comprises the following steps: (1) adding methanol, o-nitrotoluene, a catalyst, concentrated sulfuric acid, distilled water into an autoclave, performing heating with stirring to 50 DEG C, evacuating air and then introducing hydrogen, controlling a pressure in the autoclave to 0.1 MPa, carrying out a reaction for 5 h, then performing suction filtration, distilling a filtrate to remove methanol, diluting a residual solution by adding water and then adjusting pH to be neutral with ammonia water, performing extracting with toluene, washing an organic phase with a dilute sodium hydroxide solution, and performing reduced pressure distillation on the organic phase to obtain 4-methoxy-2-methylaniline; and (2) adding 4-methoxy-2-methylaniline, phenol naphthalene, cyclohexanone, and the catalyst into an autoclave, replacing air with nitrogen, performing heating to 250 DEG C, controlling a pressure in the autoclave to 1 Mpa, performing cooling to room temperature after a reaction is completed, filtering a reaction solution, and performing reduced pressure distillation on a filtrate and collecting various fractions, wherein a latter fraction is DPA. The raw materials are cheap and easy to obtain, the operation is simple, the yield is high, the energy consumption is low, and the method has practical value and economic value, andis suitable for enterprise production.
