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

A technology of dimethyl and butanol, applied in hydrolysis preparation, organic chemistry, etc., can solve the problems of high conversion rate, lower reaction yield, difficult post-processing, etc., and achieve the goals of easy availability of raw materials, high product purity, and cost reduction Effect

Active Publication Date: 2012-07-18
NANTONG CHANGHAI FOOD ADDITIVE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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
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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 reaction and produce violent reflux, after the reflux is stable, add dropwise the mixed solution of 106.6g (1mol) neopentane chloride and 450ml ether solvent tetrahydrofuran, the dropping process keeps reflux, dropwise Adding time is 50 minutes, after dropwise addition, keep reflux for 4 hours again, and gained reaction solution is Grignard reagent neopentylmagnesium chloride;

[0026] ②Cool the reaction liquid Grignard reagent neopentylmagnesium chloride prepared in step ① to 20°C, pass in dry formaldehyde gas and control the ventilation speed to ...

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 120ml of ether solvent anhydrous ether to immerse the magnesium powder, and heat After reaching 30°C, add 0.5g initiator iodine to initiate the reaction and produce violent reflux. After the reflux is stable, add dropwise the mixed solution of 106.6g (1mol) neopentane chloride and 400ml ether solvent anhydrous diethyl ether. Reflux, the dropwise addition time is 50 minutes, after dropwise addition, keep reflux for 5 hours again, the gained reaction solution is Grignard reagent neopentylmagnesium chloride;

[0033] ②Cool the reaction liquid Grignard reagent neopentylmagnesium chloride prepared in step ① to 20°C, pass in dry formaldehyde gas and control the ventilation speed to k...

Embodiment 3

[0039] Prepare 3, the concrete preparation steps of 3-dimethyl-1-butanol are as follows:

[0040] 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 methyl tetrahydrofuran to immerse the magnesium powder, heat After reaching 45°C, add 0.5g of initiator iodine to initiate the reaction and produce a violent reflux. After the reflux is stable, add dropwise the mixed solution of 151g (1mol) bromoneopentane and 500ml methyl 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 neopentylmagnesium bromide;

[0041] ②Cool the reaction liquid Grignard reagent neopentylmagnesium bromide prepared in step ① to 10°C, pass in dry formaldehyde gas and contro...

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Abstract

The invention relates to a method for preparing 3,3-dimethyl-1-butanol, which comprises the following steps of: conducting Grignard reaction by adopting formaldehyde and a Grignard reagent; and conducting hydrolysis, extraction separation and distillation on a obtained product to obtain the 3,3-dimethyl-1-butanol. According to the invention, common low-cost materials (such as halogenated neopentane, magnesium, an ether solvent and formaldehyde) can be used, the yield and purity of obtained 3,3-dimethyl-1-butanol are improved, the reaction steps and postprocessing procedures of the product are reduced, industrial production is easy to realize, and a cheap and reliable material is provided for developing 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 Applications(China)
IPC IPC(8): C07C31/125C07C29/09
Inventor 王立成蔡亚张振宇丁力陆文龙杨扬
Owner NANTONG CHANGHAI FOOD ADDITIVE
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