Catalyst, preparation method thereof and preparation method of amide compound

A technology of amide compounds and catalysts, applied in the field of catalyst preparation, which can solve the problems of restricting large-scale applications, large catalyst usage, and narrow substrate application range

Active Publication Date: 2020-01-03
SOUTH UNIVERSITY OF SCIENCE AND TECHNOLOGY OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Amide compounds can be prepared by hydrolysis of nitrile compounds. However, the most widely used catalyst for hydration of nitrile groups to amides needs to be carried out at a higher reaction temperature when catalyzing t

Method used

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  • Catalyst, preparation method thereof and preparation method of amide compound
  • Catalyst, preparation method thereof and preparation method of amide compound
  • Catalyst, preparation method thereof and preparation method of amide compound

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preparation example Construction

[0059] see figure 1 , the preparation method of the catalyst of one embodiment, comprises the following steps:

[0060] S110, reacting the precursor and the first ligand in the first solvent at 20° C. to 80° C. to obtain an intermediate.

[0061] In one embodiment, the step of mixing the precursor and the first ligand in the first solvent at 20°C to 80°C to obtain the intermediate specifically includes:

[0062] S111. Dissolving the precursor and the first ligand in the first solvent and mixing them at 20° C. to 80° C. to obtain a first reaction solution.

[0063] In one embodiment, the precursor is selected from at least one of (1,5-cyclooctadiene)platinum chloride and (1,5-cyclooctadiene)platinum bromide.

[0064] In one of the embodiments, the first ligand is selected from 1,1'-bis(diphenylphosphino)ferrocene, 1,1'-bis[(5-methyl-2-furyl)phosphino] Ferrocene, (-)-1,1-bis((2S,4S)-2,4-diethylphosphino)ferrocene, (-)-1,1-bis((2S,5S)-2 ,4-Dimethylphosphino)ferrocene, (1R)-1[...

Embodiment 1

[0121] The preparation method of the catalyst of the present embodiment is as follows:

[0122] Dissolve (1,5-cyclooctadiene)platinum chloride and 1,1'-bis(diphenylphosphino)ferrocene in dichloromethane at a molar ratio of 1:1, and then proceed at 25°C Stirring for 12 hours to obtain the first reaction solution, filtering the first reaction solution to obtain a filtrate, and distilling the filtrate under reduced pressure to obtain a solid, dissolving the solid in dichloromethane, then adding n-hexane to it for recrystallization to obtain an intermediate, The volume ratio of dichloromethane to n-hexane is 1:1; the intermediate obtained above, dimethyl hydroxyphosphine and silver tetrafluoroborate are dissolved in dichloromethane, and then stirred at 25°C for 12h to obtain the second reaction liquid, wherein the molar ratio of the intermediate to dimethylhydroxyphosphorus is 1:1.05, and the molar ratio of the intermediate to silver tetrafluoroborate is 1:1; the second reaction l...

Embodiment 2

[0132] The preparation method of the catalyst of the present embodiment is as follows:

[0133] Dissolve (1,5-cyclooctadiene)platinum chloride and 1,1'-bis[(5-methyl-2-furyl)phosphino]ferrocene in dichloro In methane, stirred at 40°C for 4h to obtain the first reaction solution, filtered the first reaction solution to obtain a filtrate, and distilled the filtrate under reduced pressure to obtain a solid, dissolved the solid in dichloromethane, and then added N-hexane is recrystallized to obtain an intermediate, and the volume ratio of dichloromethane to n-hexane is 1:1; the intermediate obtained above, dimethyl hydroxyphosphine and silver trifluoromethanesulfonate are dissolved in dichloromethane, and then Stir at 40°C for 4h to obtain a second reaction solution, wherein the molar ratio of the intermediate to dimethylhydroxyphosphorus is 1:1.05, and the molar ratio of the intermediate to silver tetrafluoroborate is 1:1; the second reaction Liquid is filtered to obtain filtrat...

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Abstract

The invention relates to a catalyst, a preparation method thereof, and a preparation method for hydrating nitrile groups into amides. The catalyst is used for catalyzing nitrile groups to be hydratedinto amides, and the structural general formula of the catalyst is shown in the specification. In the formula, a plurality of R<1> are respectively and independently ones selected from aromatic groups, heteroaromatic groups and non-aromatic ring groups; a plurality of R<2> are ones respectively and independently selected from linear alkyl groups and alkane aromatic groups; X is one selected from Cl and Br; and L is one selected from OTf, BF4, PF6 and SbF6. The catalyst can catalyze nitrile groups to be hydrated into amides, and the nitrile groups can be catalyzed to be hydrated into amides even at a low temperature (20-80 DEG C); besides, compared with existing common catalysts for catalyzing nitrile groups to be hydrated into amides, the catalyst has the advantages that the equivalent weight of the catalyst can be obviously reduced, and nitrile groups can reach a relatively high conversion rate when the equivalent weight of the catalyst is only 0.01 mol%-0.5 mol%; and meanwhile, the catalyst is wider in application range and can catalyze various nitrile compounds to be hydrated into amide compounds.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a catalyst, a preparation method thereof, and a preparation method of an amide compound. Background technique [0002] Amide compounds are a very important class of organic compounds, which can be used not only as structural units of physiologically active natural products, but also widely used in the synthesis of some pharmaceutical intermediates. Amide compounds can be prepared by hydrolysis of nitrile compounds. However, the most widely used catalyst for hydration of nitrile groups to amides needs to be carried out at a higher reaction temperature when catalyzing the hydration of nitrile groups into amides, and the amount of catalyst used At the same time, the scope of application of the substrate is narrow, and there are relatively large limitations, which limit its large-scale application. Contents of the invention [0003] Based on this, it is necessary to p...

Claims

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Application Information

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IPC IPC(8): C07F19/00B01J31/24C07C231/06C07D213/87C07D307/68C07D333/38C07F17/02C07C233/03C07C233/11C07C233/65C07C235/06C07C233/58C07B43/06
CPCC07F17/02B01J31/2409C07C231/06C07D333/38C07D307/68C07D213/87C07B43/06B01J2231/641C07C233/03C07C233/11C07C233/65C07C235/06C07C233/58
Inventor 邢祥友徐晨陈波
Owner SOUTH UNIVERSITY OF SCIENCE AND TECHNOLOGY OF CHINA
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