Method for preparing organic phosphonic gold chloride (I) compound

A compound, gold chloride technology, applied in the field of compound preparation, can solve problems that are not green, efficient, and safe production methods, and achieve the effects of cost controllable, safe preparation methods, and efficient production

Active Publication Date: 2016-08-17
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Use thiodialkyl compounds or derivatives thereof to promote the reaction of tetrachloroauric acid and its salts with phosphine-containing ligands as reducing agents, because the adopted thiodialkyl compounds or derivatives thereof usually or have a strong Irritant odor, or mustard gas raw materials for chemical weapons are subject to the control of relevant departments, they are undoubtedly not green, efficient and safe production methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A kind of preparation method of organic phosphine gold chloride (I) compound, comprises the steps:

[0033] (1) 2g (4.83mmol) KAuCl 4 2H 2 Add O into a 250mL reaction bottle, add 50mL distilled water to dissolve, and stir evenly with a magnetic stirrer in an ice-water bath (0°C).

[0034] (2) Keep the temperature of ice water in the reaction vessel in step (1), and slowly add 3.16g (14.5mmol) within 45 minutes (add 1 / 9 of the sample amount every 5 minutes, and finish adding within 45 minutes) 4,4 '-Thiodiphenol, stir evenly with a rotating speed of 1200~1400 rpm, the color of the solution changes from yellow to brown and finally to purple.

[0035] (3) Prepare a mixture of 1.27g (4.83mmol) triphenylphosphine and 48.3mL ethanol, add the mixture containing phosphine ligand and ethanol dropwise into the reaction vessel of step (2), remove the ice-water bath, Naturally return to room temperature (20°C) and magnetically stir for 2 hours.

[0036] (4) Stop stirring after ...

Embodiment 2

[0041] A kind of preparation method of organic phosphine gold chloride (I) compound, comprises the steps:

[0042] (1) 200mg (0.48mmol) KAuCl 4 2H 2 Add O into a 25mL reaction bottle, add 5mL distilled water to dissolve, and stir evenly with a magnetic stirrer in an ice-water bath (0°C).

[0043] (2) Keep the temperature of ice water in the reaction vessel in step (1), slowly add 0.24mL (1.44mmol) of diphenylsulfide within 45 minutes (add 1 / 9 of the sample volume every 5 minutes, and finish adding within 45 minutes) Ether was stirred evenly at a speed of 330 rpm, and the color of the solution was yellow-red.

[0044] (3) Prepare a mixture of 127mg (0.48mmol) triphenylphosphine and 5mL ethanol, add the mixture of phosphine-containing ligand and ethanol dropwise into the reaction vessel of step (2), remove the ice-water bath, and recover naturally to room temperature (20°C) and stirred magnetically for 3 hours.

[0045] (4) (same as embodiment 1).

[0046] (5) (same as Exam...

Embodiment 3

[0050] A kind of preparation method of organic phosphine gold chloride (I) compound, comprises the steps:

[0051] (1) 500mg (1.21mmol) KAuCl 4 2H 2 Add O into a 50mL reaction bottle, add 12mL distilled water to dissolve, and stir evenly with a magnetic stirrer in an ice-water bath (0°C).

[0052](2) Keep the temperature of ice water in the reaction vessel in step (1), slowly add 730 mg (3.63 mmol) of 2-benzenesulfide within 45 minutes (add 1 / 9 of the sample amount every 5 minutes, and finish adding within 45 minutes) Aniline, stirred evenly with a rotating speed of 330 rpm, the color of the solution was dark green.

[0053] (3) Prepare a mixture of 316mg (1.21mmol) triphenylphosphine and 12mL ethanol, add the mixture of phosphine-containing ligand and ethanol dropwise into the reaction vessel of step (2), remove the ice-water bath, and recover naturally to room temperature (20°C) and stirred magnetically for 3 hours.

[0054] (4) (same as embodiment 1).

[0055] (5) (sam...

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PUM

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Abstract

The invention discloses a method for preparing an organic phosphonic gold chloride (I) compound. The method comprises the following steps: (1) adding chloroauric acid hydrated salt into a reaction container, dissolving with water, and uniformly stirring in an ice-water bath; (2) keeping the temperature of the ice water in the reaction container, dripping a glucosinolates diaryl compound or a derivative of the glucosinolates diaryl compound, and stirring uniformly; (3) dripping a mixed liquid of phosphine-containing ligand and ethanol into the reaction container one droplet by one droplet, removing the ice-water bath, recovering the room temperature naturally, and stirring for 2-5 hours; (4) stopping stirring, performing suction filtration, washing with cold methanol, dissolving the collected solid with an organic solvent, and performing suction filtration again so as to remove insoluble matters; (5) performing concentration spinning drying on the solution, recrystallizing with a solvent, and performing suction filtration again, thereby obtaining the organic phosphonic gold chloride (I) compound. As the glucosinolates diaryl compound or the derivative of the glucosinolates diaryl compound is taken as a reduction reagent, and due to reaction between the chloroauric acid hydrated salt and the phosphine-containing ligand in an ethanol-water system, environment-friendly, safe and efficient production of the organic phosphonic gold chloride (I) compound can be achieved, and moreover, industrial application of the organic phosphonic gold chloride (I) compound is facilitated.

Description

technical field [0001] The invention relates to the technical field of compound preparation, in particular to a method for preparing an organic phosphine gold(I) chloride compound which is green, efficient and convenient for industrialization. Background technique [0002] Gold catalysts are used in metal-organic reactions, and have made great progress in the fields of carbon-carbon bond coupling, catalytic hydrogenation, and hydrocarbon activation. At the beginning of the 21st century, gold catalysts began to be used in sugar chemistry, especially glycosylation reactions, and achieved rapid development. In addition, triphenylphosphine gold chloride and its analogues have been found to have the function of inducing apoptosis of cancer cells, have the potential to be developed into anticancer drugs, and have good biological application prospects in inhibiting the growth of melanoma cells. [0003] At present, the preparation of organophosphine gold(I) chloride compounds is m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/50C07F19/00C07F1/12
CPCC07F1/005C07F9/5022C07F9/505C07F17/02
Inventor 杨友王骏畅
Owner EAST CHINA UNIV OF SCI & TECH
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