3217-86-5Relevant articles and documents
PRODUCTION METHOD OF AMIDE COMPOUND
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Paragraph 0134-0137, (2020/10/08)
PROBLEM TO BE SOLVED: To provide a production method of an amide compound, which can use a variety of carboxylic acid halides and can produce a desired amide compound at a yield higher than a batch process by suppressing a side reaction. SOLUTION: Provided is a production method of an amide compound using a flow type reactor, in which the flow type reactor includes: a first flow path; a second flow path; a first mixing means provided at a confluent part of the first flow path and the second flow path; and a third flow path that is connected to the first mixing means and arranged on a down stream side of the first mixing means, the production method comprising: a mixing step of obtaining a mixed liquid by circulating a first liquid containing the carboxylic acid halide in the first flow path, circulating a second liquid containing an amine compound having a molecular weight of 1,000 or less, an inorganic alkali and water in the second flow path, and mixing the first liquid and the second liquid by the first mixing means to obtain a mixture; and a reaction step of obtaining an amide compound by circulating the mixed liquid in the third flow path and reacting the carboxylic acid halide and the amine compound in the third flow path. SELECTED DRAWING: Figure 1 COPYRIGHT: (C)2020,JPO&INPIT
HOMOGENOUS PROCESS FOR THE HYDROGENATION OF CARBOXYLIC ACIDS AND DERIVATIVES THEREOF
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Page/Page column 13, (2008/06/13)
A homogenous process for the hydrogenation of the carboxylic acids and/or derivatives thereof in the presence of a catalyst comprising ruthenium, rhodium, iron, osmium or palladium, and an organic phosphine is described in which the hydrogenation is carried out in the presence of at least about 1% by weight water. A process for regenerating a catalyst comprising ruthenium, rhodium, iron, osmium or palladium and an organic phosphine is also described in which the regeneration is carried out in the presence of hydrogen and water.
Multigram Preparation of 2-Alkylpyrimidines in the Vapor Phase from Carboxylic Acids and 1,3-Diaminopropane over a Dual Catalyst System
Hull, John W.,Otterson, Kari
, p. 2925 - 2929 (2007/10/02)
2-Alkylpyrimidines 2 were obtained from cofeeding a carboxylic acid such as pivalic acid (3a) or propionic acid (3b) and 1,3-diaminopropane (4) over first an alumina catalyst at 250-290 deg C and second a palladium dehydrogenation catalyst at 300-340 deg C to give 2 directly in 56-68percent overall yields.On the alumina bed, initial amidation of organic acid occurs to give the monoacyltrimethylenediamine 5, followed by ring closure to the tetrahydropyrimidine intermediate 6.An equilibrium between 5, 6, and water is established on the alumina bed, with an apparent equilibrium constant of 53 +/- 7 mol/kg at 290 deg C.The high temperature of the alumina bed shifts the equilibrium in favor of 6, which is directly dehydrogenated to 2 over the palladium catalyst.The method avoids the need to isolate and purify solid intermediates.The presence of low levels of sulfur acts as a strong palladium catalyst deactivator.Gradual decline of palladium catalyst activity was observed due to carbon buildup.No decline in alumina catalyst activity was observed.The continuous process allows for the preparation of multigram quantities of 2 with a laboratory-scale reactor.
