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Method for synthesizing alpha-hydroxyketone intermediate by using supported catalyst

A technology of supporting catalysts and hydroxy ketones, which is applied in the field of supporting catalysts to synthesize α-hydroxy ketone intermediates. It can solve the problems of unrecyclable prices, unsafe use, and high cost of three products, and achieves simple operation, good dispersion, and high yield. The effect of high purity

Inactive Publication Date: 2019-04-19
交城县兆晨煤焦有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention is to solve the catalyst AlCl used in the preparation method of existing α-hydroxy ketone intermediate 3 , large amount, high cost, non-recyclable, and other Lewis catalysts are expensive and unsafe to use. A method for synthesizing α-hydroxyketone intermediates with supported catalysts is provided. Anhydrous AlCl 3 Loading on different carriers to obtain supported AlCl 3 , so that it has good regeneration performance and environmental friendliness

Method used

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  • Method for synthesizing alpha-hydroxyketone intermediate by using supported catalyst
  • Method for synthesizing alpha-hydroxyketone intermediate by using supported catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] AlCl 3 / Chitin, AlCl 3 / Synthesis of acetylated chitin

[0033] Put 200g of chitin that has been ground, washed with acid and alkali, washed with water and alcohol and dried (vacuum-dried for 1d at 100°C) into a 5000mL three-necked flask, add 3000ml of dried chloroform, and under the protection of argon, add 90g of Aluminum trichloride in water, react at 60°C for 3 days, cool to room temperature, filter under the protection of argon, vacuum dry at 80°C for 4 hours, and store in an argon atmosphere box.

[0034] In the same way, AlCl can be made 3 / Acetylated chitin.

[0035] where AlCl 3 / Chitin, AlCl 3 The loads of acetylated chitin were 2.58mmol / g and 2.24mmol / g.

Embodiment 2

[0037] Cyclohexyl phenyl ketone (AlCl 3 / chitin catalyzed) synthesis

[0038] Take by weighing the 7.75g AlCl that embodiment 1 prepares 3 / chitin (20mmol) into a 100ml three-necked flask, under argon protection, add cyclohexylformyl chloride (18mmol) and benzene (90mmol), cool to 10°C, then heat up to 25°C, GC or TLC to detect the progress, the reaction is over Finally, filter, and the filtrate is treated with 100ml of ice water, separated into layers, washed with water and neutralized, dried over anhydrous sodium sulfate, filtered, distilled with low boiling point substances, and then further rectified to obtain the product.

[0039] The nuclear magnetic spectrum data of gained product is:

[0040] 1 HNMR (400MHz, CDCl 3 ):δ7.93(d,2H),7.55-7.48(m,H),7.49-7.41(m,2H),

[0041] 3.31-3.20 (m, 1H), 1.92-1.77 (m, 4H), 1.78-1.70 (m, 1H), 1.56-1.22 (m, 5H).

Embodiment 3

[0043] Cyclohexyl phenyl ketone (AlCl 3 / acetylated chitin catalyzed) synthesis

[0044] Take by weighing the 8.93g AlCl that embodiment 1 prepares 3 / Acetylated chitin (20mmol) was put into a 100ml three-necked flask, under argon protection, added cyclohexylformyl chloride (18mmol) and benzene (90mmol), cooled to 10°C, then heated to 35°C, GC or TLC to detect the progress, After the reaction, filter, and the filtrate is treated with 100ml of ice water, separated into layers, washed with water and neutralized, dried with anhydrous sodium sulfate, filtered, distilled with low boiling point substances, and then further rectified to obtain the product.

[0045] The nuclear magnetic spectrum data of gained product is:

[0046] 1 HNMR (400MHz, CDCl 3 ):δ7.90(d,2H),7.56-7.49(m,H),7.51-7.40(m,2H),

[0047] 3.30-3.19 (m, 1H), 1.91-1.76 (m, 4H), 1.77-1.68 (m, 1H), 1.54-1.20 (m, 5H).

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Abstract

The invention relates to the technical field of organic synthesis, specifically to a method for synthesizing an alpha-hydroxyketone intermediate by using a supported catalyst, in particular to a method for preparing an aromatic compound and an acyl chloride by using an aluminum trichloride supported catalyst. The preparation method provided by the invention avoids the direct use of anhydrous aluminum trichloride, avoids a large amount of aluminum-containing acidic wastewater brought by the post-reaction treatment, simplifies the process, has simple process operation, and meets the trend of green large-scale production under increasingly stringent environmental protection.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing an alpha-hydroxy ketone intermediate with a supported catalyst. Background technique [0002] α-Hydroxy ketones are the main components of UV-curable materials and are widely used in many fields such as electronics, optical fiber, printing, packaging, adhesives, coatings and composite materials. Its representative products include 1173, 184, 651 and 2959, etc. These products are widely used in UV curing materials due to their high initiation efficiency, high solubility, low odor, low pollution, good stability, and yellowing resistance. [0003] Usually, anhydrous aluminum trichloride is used as a catalyst for the intermediates in the preparation of α-hydroxy ketones. After the reaction, the system becomes homogeneous, and it is necessary to add glacial hydrochloric acid solution to the reaction liquid for washing to decompose aryl ketone-tri A...

Claims

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Application Information

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IPC IPC(8): B01J31/26C07C45/46C07C49/792C07C49/76
CPCB01J31/26B01J2231/4205C07C45/46C07C2601/14C07C49/792C07C49/76
Inventor 王福泉
Owner 交城县兆晨煤焦有限公司
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