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Method for preparing 3,3-dimethyl butyraldehyde

A technology of dimethyl butyraldehyde and dimethyl butyryl chloride, which is applied in 3 fields, can solve the problems of serious environmental pollution, low yield, and large amount of hydrogen, and achieve high purity, high product yield, and low production cost Effect

Inactive Publication Date: 2011-04-13
太仓浦源医药原料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0015] This method reacts with hydrogen gas at normal pressure, and the reaction conditions are relatively mild, but a large amount of hydrogen chloride acid gas is discharged to the atmosphere, which seriously pollutes the environment, and the amount of all hydrogen gas is large, and the yield is not high.

Method used

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  • Method for preparing 3,3-dimethyl butyraldehyde
  • Method for preparing 3,3-dimethyl butyraldehyde
  • Method for preparing 3,3-dimethyl butyraldehyde

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Take a 10L high-pressure hydrogenation reactor and replace it with high-purity nitrogen three times, add 1L 3,3-dimethylbutyryl chloride, 3L anhydrous toluene, 20g 10% Pd / C, 1.2kg potassium carbonate, 40g CeCl 3 , Tighten the reaction kettle, replace it with high-purity nitrogen three times and high-purity hydrogen three times in sequence, control the pressure inside the kettle to 40psi, stir at 1000 rpm, slowly raise the temperature to 130°C, react for about 2 hours, and no longer absorb hydrogen to indicate the reaction complete. After cooling down to room temperature, replace it with nitrogen three times, filter and recover Pd / C, collect the 100-105°C fraction of the filtrate with a rectification column, and obtain 680g of the product, with a yield of 94% and a GC of 98.7%.

Embodiment 2

[0032] Take a 10L high-pressure hydrogenation reactor and replace it with high-purity nitrogen three times, add 1.5L 3,3-dimethylbutyryl chloride, 3L anhydrous dioxane, 40g 10% Pt / C, 950g anhydrous pyridine, 60g CuCl, twist The reaction kettle was replaced three times with high-purity nitrogen and three times with high-purity hydrogen in sequence. The pressure inside the kettle was controlled at 25 psi, the stirring speed was 1000 rpm, and the temperature was slowly raised to 120 ° C. The reaction was about 1.5 hours. If no more hydrogen was absorbed, the reaction was complete. After cooling down to room temperature, replace with nitrogen three times, filter and recover Pt / C, wash the filtrate with 10L of 5% salt water to remove the solvent, and rectify the obtained oily product with a rectification column, collect fractions at 100-105°C, and obtain 970g of the product with a yield of 90%, GC99 .2%.

Embodiment 3

[0034] Take a 10L high-pressure hydrogenation reactor and replace it with high-purity nitrogen three times, add 1.5L 3,3-dimethylbutyryl chloride, 4L ethylene glycol dimethyl ether, 60g 5% Pd / C, 1kg lithium carbonate, 50g MgCl 2 , Tighten the reactor, replace it with high-purity nitrogen three times and high-purity hydrogen three times in turn, control the pressure inside the kettle to 60 psi, stir at 1000 rpm, slowly raise the temperature to 100°C, react for about 4 hours, and no longer absorb hydrogen to indicate the reaction complete. After cooling down to room temperature, replace with nitrogen three times, filter to recover Pd / C, wash the filtrate with 15L of 5% brine, and collect the 100-105°C fraction of the oily product with a rectification column to obtain 950g of the product, with a yield of 88% and a GC of 99.0%.

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Abstract

The invention provides a method for preparing 3,3-dimethyl butyraldehyde, which comprises the following steps of: adding an acid-binding agent, a catalyst, an auxiliary catalyst and a solvent into 3,3-dimethyl butyryl chloride, and reacting under a certain pressure of H2 to obtain the 3,3-dimethyl butyraldehyde, wherein the acid-binding agent is from inorganic base or organic base; the catalyst is selected from recyclable precious metals; and the auxiliary catalyst is a metal salt. The method is suitable for the large-scale industrial production of the 3,3-dimethyl butyraldehyde; in the method, the raw materials used are cheap and readily available, the drawback that a large amount of hydrogen is discharged into the atmosphere in a normal-pressure reaction is overcome; and the method is environmentally-friendly; the reaction is compete, the product yield and product purity are high, the post treatment is simple and the production cost is low.

Description

technical field [0001] The invention relates to 3,3-dimethylbutyraldehyde, in particular to a preparation method of 3,3-dimethylbutyraldehyde. Background technique [0002] Neotame is a new type of dipeptide strong sweetener, which is a derivative of aspartame. Its stability and use cost are better than aspartame, and it has attracted the attention of the world's food industry since it came out. . In July 2002, FDA officially approved the use of neotame in food. China also approved the use of neotame in various foods in April 2003, and added it according to production needs. 3,3 dimethylbutyraldehyde is an important intermediate for the synthesis of neotame, and its purity and cost directly affect the purity of sweetness and price of neotame. [0003] Existing synthetic 3, the method for 3-dimethylbutyraldehyde (DMBA) mainly contains: [0004] Method 1: Isobutylene Ethylene Acid Hydration Oxidation Method (Please refer to Patent No. US 6,573,409, the date of authorizatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/02C07C45/41
CPCY02P20/584
Inventor 周富荣周伟锋邵林华
Owner 太仓浦源医药原料有限公司
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