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Reaction device suitable for aldol reaction

A reaction device and reaction technology, applied in the preparation of organic compounds, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve problems such as no use value, achieve low cost, convenient separation, simple and easy to operate Effect

Active Publication Date: 2011-06-22
SUZHOU HAOLI CULTURE MEDIA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If both reactants have active α-hydrogens, four mixed products will be obtained. If the products are difficult to separate, this is of little use value.

Method used

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  • Reaction device suitable for aldol reaction
  • Reaction device suitable for aldol reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment one: see figure 1 , Preparation of proline-loaded silica catalyst

[0029] Disperse 100ml, 300-400 mesh silica gel powder in acidic solution, stir at 60-70°C for 12h, then cool, treat, then disperse in solvent, add 7mL 3-aminopropyl at 40-60°C Triethoxysilane, stirred steadily for 12h, then added 2g of proline into the solution, kept stirring for 4-8h.

Embodiment 2

[0030] Embodiment 2: Construction of catalytic device

[0031] Synthesize the silica gel powder connected with proline according to the claim, put the silica gel powder into the chromatographic column, and then pressurize the silica gel to overfill evenly, then add a sufficient amount of ethanol to remove the proline that is not connected to the silica gel Rinse it down and set aside.

Embodiment 3

[0032] Example 3: Catalyzing different aldehyde and ketone compounds for Aldol reaction experiments

[0033] Operation process: Pour the aldehyde and ketone mixed solution (raw material 1 and raw material 2) mixed in a certain proportion into the chromatography column, rely on gravity to flow down naturally, and after the liquid is completely flowed out, pour the collected solution into the obtained solution in Example 2 Chromatographic column, repeated three times. Then take a sample and carry out GC to measure the composition and the productive rate of the reactant, and the results are shown in Table 1.

[0034] The test instrument is a gas chromatograph with a hydrogen flame detector, and the sample gas is the cylinder standard gas.

[0035] Chromatography conditions: host: GC-2014 gas chromatograph; column: 5A molecular sieve packed column; column temperature: 100°C, detector temperature: 300°C.

[0036] Table 1 Aldol reaction results of different raw materials

[0037]...

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Abstract

The invention belongs to the field of an aldol reaction device, and relates to a chromatographic column which can be used for fixing a catalytic agent on a stationary phase, wherein the chromatographic column is a reaction device suitable for aldol reaction. The reaction device is the chromatographic column, the stationary phase in the chromatographic column is silicon dioxide, the surface of thesilicon dioxide is connected with catalytic agent praline, and a coupling agent which connects the silicon dioxide and the catalytic agent praline is 3-azyl propyltriethoxysilane. The catalytic agentis fixed on the stationary phase, and mobile-phase reaction raw materials can repeatedly flow through the catalytic agent, so that the reaction can be completely performed; and the catalytic agent can not be retained in a reaction product, so that the reaction product can be conveniently separated.

Description

technical field [0001] The invention belongs to the field of aldol reaction devices, and relates to a chromatographic column for fixing a catalyst on a stationary phase, and the chromatographic column is a reaction device suitable for aldol reaction. Background technique [0002] The aldol reaction gets its name from the reaction product aldol, or hydroxyaldehyde. The earliest discovered aldol reaction is the aldol reaction between acetaldehyde molecules, and the product is an aldehyde with a hydroxyl group, so it is called the aldol reaction. In addition to aldehydes, ketones, esters, amides, etc. can also undergo aldol reactions. [0003] The aldol reaction is simply a reaction between two aldehyde or ketone molecules. As shown in the following reaction formula: [0004] ; [0005] Under alkaline conditions, two molecules of acetaldehyde interact to form a new carbon-carbon bond to generate product a, namely β-hydroxybutyraldehyde. When the reaction is carried out a...

Claims

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Application Information

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IPC IPC(8): B01J8/02B01J20/22B01J20/30B01J20/28B01D15/22C07C49/245C07C45/73C07C205/45C07C201/12C07C255/56C07C253/30C07C49/255C07C49/403
Inventor 顾宏伟李敏路建美曹雪琴
Owner SUZHOU HAOLI CULTURE MEDIA TECH CO LTD
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