Method for preparing 3,3-dimethyl-1-butanol

A technology of dimethyl and butanol, which is applied in the preparation of hydroxyl compounds, organic compounds, chemical instruments and methods, etc., can solve the problems of difficult post-processing, reduced reaction yield, high conversion rate, etc. The effect of high product purity and cost reduction

Active Publication Date: 2014-05-28
NANTONG CHANGHAI FOOD ADDITIVE
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

Although this method raw material is easy to get, the Grignard reaction that Grignard reagent tert-butylmagnesium halide and 1,2-dihaloethanes carry out involves a lot of side reactions, especially Grignard reagent will be mixed with 1,2-dihaloethanes. The second halogen atom of the alkane undergoes a coupling reaction to generate macromolecular 2,2,5,5-tetramethylhexane, thereby reducing the yield of the reaction and causing difficulties in post-processing, and after the Grignard reaction , 3,3-dimethyl-1-halo-butane is hydrolyzed while side reactions such as elimination reactions exist, the conversion rate will be high, but the yield of the product will not be high

Method used

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  • Method for preparing 3,3-dimethyl-1-butanol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Prepare 3, the concrete preparation steps of 3-dimethyl-1-butanol are as follows:

[0025] ①In a 1000ml four-neck flask equipped with a thermometer, reflux condensing device, drying device, dropping device, and stirring device, add 26.4g (1.1mol) of magnesium powder, and at the same time add 100ml of ether solvent tetrahydrofuran to immerse the magnesium powder, and heat to 45 After ℃, add 3g initiator bromoethane to initiate the reaction and produce violent reflux. After the reflux is stable, add dropwise the mixed liquid of 92.5g (1mol) chlorobutane and 400ml ether solvent tetrahydrofuran, and keep the reflux during the dropping process. Adding time is 45 minutes, after the dropwise addition is completed, keep refluxing for 3.5 hours, and the resulting reaction solution is Grignard reagent tert-butylmagnesium chloride;

[0026] ② Cool the reaction liquid Grignard reagent tert-butylmagnesium chloride prepared in step ① to 20°C, feed ethylene oxide gas and control the v...

Embodiment 2

[0031] Prepare 3, the concrete preparation steps of 3-dimethyl-1-butanol are as follows:

[0032] ① Add 27.6g (1.15mol) of magnesium powder into a 1000ml four-necked flask equipped with a thermometer, reflux condensing device, drying device, dropping device, and stirring device, and at the same time add 100ml of ether solvent anhydrous ether to immerse the magnesium powder, and heat After reaching 35°C, add 0.5g initiator iodine to initiate the reaction and produce a violent reflux. After the reflux is stable, add dropwise a mixed liquid of 92.5g (1mol) chlorobutane and 400ml ether solvent diethyl ether, and keep the reflux during the dropping process. The dropwise addition time is 50 minutes, after the dropwise addition is completed, keep refluxing for 5 hours, and the resulting reaction solution is Grignard reagent tert-butylmagnesium chloride;

[0033] ② Cool the reaction liquid Grignard reagent tert-butylmagnesium chloride prepared in step ① to 20°C, feed ethylene oxide ga...

Embodiment 3

[0038] Prepare 3, the concrete preparation steps of 3-dimethyl-1-butanol are as follows:

[0039] ①In a 1000ml four-neck flask equipped with a thermometer, reflux condensing device, drying device, dropping device, and stirring device, add 27.6g (1.15mol) of magnesium powder, and at the same time add 100ml of ether solvent tetrahydrofuran to immerse the magnesium powder, and heat to 45 After ℃, add 0.5g initiator iodine to initiate the reaction and produce violent reflux. After the reflux is stable, add dropwise the mixed liquid of 137g (1mol) bromo-tert-butane and 400ml ether solvent tetrahydrofuran. For 45 minutes, after the dropwise addition was completed, it was kept under reflux for 3.5 hours, and the resulting reaction solution was Grignard reagent tert-butylmagnesium bromide;

[0040] ② Cool the reaction liquid Grignard reagent tert-butylmagnesium bromide prepared in step ① to 10°C, feed ethylene oxide gas and control the ventilation speed to keep the temperature of the re...

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Abstract

The invention relates to a method for preparing 3,3-dimethyl-1-butanol. The method comprises the following steps of: enabling ethylene oxide and a Grignard reagent to perform a Grignard reaction, and carrying out hydrolyzation, extraction separation and distillation on products obtained from the Grignard reaction to obtain the 3,3-dimethyl-1-butanol. According to the method disclosed by the invention, conventional low-cost raw materials (such as halogenated ter-butane, magnesium, an ether solvent and the ethylene oxide) can be utilized, and the prepared 3,3-dimethyl-1-butanol has improved yield and purity, reaction steps and a post-treatment process of the 3,3-dimethyl-1-butanol are reduced, the industrial production is more easy to realize, and a cheaper and more reliable raw material, namely the 3,3-dimethyl-1-butanol is provided for development of a novel food additive, namely, neotame.

Description

technical field [0001] The invention relates to a preparation method of 3,3-dimethyl-1-butanol. Background technique [0002] Neotame is a new type of food additive, its sweetness is 8,000 times that of sucrose, so it has attracted attention. The main intermediate in the synthesis of neotame, 3,3-dimethylbutyraldehyde, is produced by oxidation of 3,3-dimethyl-1-butanol. Chinese patent CN101696153A discloses using halogenated tert-butane and 1,2-dichloroethane, or 1,2-dibromoethane, or 1,2-diiodoethane as raw materials to first prepare tert-butylmagnesium halide Grignard reagent, then Grignard reaction with 1,2-dihaloethane to synthesize 3,3-dimethyl-1-halo-butane, and then hydrolyzed in aqueous potassium hydroxide solution to obtain 3,3-dimethyl base-1-butanol. Although this method raw material is easy to get, the Grignard reaction that Grignard reagent tert-butylmagnesium halide and 1,2-dihaloethanes carry out involves a lot of side reactions, especially Grignard reagent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/125C07C29/36
Inventor 王立成蔡亚张振宇丁力陆文龙陈凯
Owner NANTONG CHANGHAI FOOD ADDITIVE
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