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Preparation method and application of dimethyl acetylacetone gold

A technology of acetylacetone and dimethyl, which is applied in the field of complex catalysis and achieves the effects of easy operation and mild conditions

Pending Publication Date: 2018-11-06
YANGZHOU POLYTECHNIC INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, to dimethyl (acetylacetonate) gold (Ⅲ) (Me 2 (acac) Au) report less, the invention provides a kind of preparation method of dimethyl (acetylacetonate) gold (III) and its application in catalytic coupling reaction

Method used

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  • Preparation method and application of dimethyl acetylacetone gold

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] (1) Dissolve gold chloride (1 mmol) in ether (10 mL), add methyl iodide (2.5 mmol), and stir at room temperature for 2 hours to obtain reaction solution A;

[0015] (2) Add potassium tert-butoxide (3mmol) to acetylacetone (3mmol) and stir at room temperature for 10min to obtain reaction solution B;

[0016] (3) Under an ice bath, mix the reaction solution A and the reaction solution B, naturally return to room temperature, stir and react for 30 minutes, dilute with ether, wash with water, and concentrate the organic layer (ether layer) under reduced pressure and vacuum dry to obtain two Methyl (acetylacetonate) gold (III) (294 mg, yield is about 90.1%, melting point 82-84°C).

Embodiment 2

[0018] (1) Dissolve gold chloride (1 mmol) in ether (15 mL), add methyl iodide (3.0 mmol), and stir at room temperature for 1 hour to obtain reaction solution A;

[0019] (2) Add potassium tert-butoxide (5 mmol) to acetylacetone (5 mmol), and stir at room temperature for 15 minutes to obtain reaction solution B;

[0020] (3) Under ice bath, mix reaction solution A and reaction solution B, return to room temperature naturally, stir and react for 40 minutes, dilute with ether, wash with water, and concentrate the organic layer (ether layer) under reduced pressure and dry in vacuo to obtain two Methyl (acetylacetone) gold (III) (301mg, yield is about 92.3%, melting point 82-84°C).

Embodiment 3

[0022]

[0023] Take compound 2 (1.2mmol) and dissolve it in DMF / H 2 O mixed solvent (DMF: H 2 O=5:1, v / v), at room temperature, add dimethyl(acetylacetone) gold (Ⅲ) (0.1mmol) and stir for 5min, add compound 1 (1.0mmol) and potassium carbonate (5mmol), continue to room temperature After stirring and reacting for 15 minutes, the reaction solution was poured into ice water to separate out solids, filtered, the filter cake was washed with water and n-hexane in turn, and dried under vacuum to obtain compound 3 (205 mg, yield is about 93.7%) 1 H NMR(400MHz, CDCl 3 ):δ7.56-7.43(m,8H,Ph- H ),4.75(s,2H,C H 2 ),1.80(s,1H,O H ).

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Abstract

The invention relates to a preparation method and application of dimethyl acetylacetone gold. The preparation method comprises the following steps: (1) dissolving gold chloride into ethyl ether, adding methyl iodide, and stirring for 1-2 hours at the room temperature so as to obtain a reaction liquid A; (2) putting potassium tert-butoxide into acetylacetone, and stirring for 10-15 minutes at the room temperature so as to obtain a reaction liquid B; (3) at ice bath, mixing the reaction liquid A with the reaction liquid B, recovering to the room temperature naturally, carrying out a stirring reaction for 30-40 minutes, diluting with the ethyl ether, washing with water, and carrying out vacuum concentration with an organic layer (an ethyl ether layer), and carrying out vacuum drying, therebyobtaining the dimethyl (acetylacetone) gold (III).

Description

Technical field [0001] The invention belongs to the field of complex catalysis, and specifically relates to a preparation method and application of gold dimethyl acetylacetonate. Background technique [0002] Acetylacetonate is widely used in chemical industry, petroleum, medicine, electronics, materials and other fields, mainly for catalysis, stabilization and promotion. For example, calcium acetylacetonate is a catalyst for the transesterification of methyl methacrylate and dimethylaminoethanol to synthesize DMA; iron acetylacetonate can be used as a high-efficiency photosensitive catalyst for the photodegradation of plastics; in addition, calcium acetylacetonate and zinc acetylacetonate are rigid PVC, etc. The heat stabilizer of halides is also the accelerator of resin hardening. In the prior art, dimethyl (acetylacetonate) gold (Ⅲ) (Me 2 (acac) Au) is less reported. The present invention provides a method for preparing dimethyl (acetylacetonate) gold (III) and its applicatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/77C07C49/92B01J31/22C07C29/34C07C33/46
CPCC07C29/34C07C45/77B01J31/2213B01J2231/4227B01J2531/18C07C49/92C07C33/46
Inventor 于晓萍王斌
Owner YANGZHOU POLYTECHNIC INST
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