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Preparation method of 3,3-dimethyl butanol

A technology of dimethyl butanol and dimethyl butyric acid is applied in the field of preparation of 3,3-dimethyl butanol, and can solve the problems of high production cost, high price, low yield and the like of dimethyl butanol , to achieve the effect of low cost, low price and high yield

Active Publication Date: 2015-10-14
GUANGXI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above processes either use flammable and explosive reagents (such as lithium aluminum hydride, etc.), solvents (such as ether, etc.), and are expensive and have low yields. The production cost of 3,3-dimethylbutanol is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Put 11.6g of 3,3-dimethylbutyric acid and 24mL of absolute ethanol into the reaction flask, stir evenly, then add 1mL of concentrated sulfuric acid, raise the temperature to about 75°C and reflux for 12h. Cool in an ice-water bath to 0-5°C, add sodium hydroxide solution to adjust the pH to about 8, slowly add 0.15 mol of sodium borohydride solution dropwise, and then raise the temperature to 75°C for 5 hours of reaction. Cool in an ice-water bath, adjust the pH value to 5-6 with dilute hydrochloric acid. Recover ethanol under reduced pressure at 40°C, add sodium chloride to the residue until saturated, extract with ethyl acetate, wash the organic layer with saturated brine, and dry over anhydrous sodium sulfate , ethyl acetate was recovered under reduced pressure to obtain 3,3-dimethylbutanol as a colorless to light yellow liquid with a yield of 90%.

Embodiment 2

[0018] Put 11.6g of 3,3-dimethylbutyric acid and 24mL of absolute ethanol into the reaction flask, stir evenly, then add 1mL of concentrated sulfuric acid, raise the temperature to about 75°C and reflux for 12h. Cool in an ice-water bath to 0-5°C, add sodium hydroxide solution to adjust the pH to about 8, slowly add 0.15 mol potassium borohydride solution dropwise, and raise the temperature to 75°C for 5 hours after the drop is complete. Cool in an ice-water bath, adjust the pH value to 5-6 with dilute hydrochloric acid. Recover ethanol under reduced pressure at 40°C, add sodium chloride to the residue until saturated, extract with ethyl acetate, wash the organic layer with saturated brine, and dry over anhydrous sodium sulfate , ethyl acetate was recovered under reduced pressure to obtain 3,3-dimethylbutanol as a colorless to light yellow liquid with a yield of 92%.

Embodiment 3

[0020] Put 11.6g of 3,3-dimethylbutyric acid and 24mL of absolute ethanol into the reaction flask, stir evenly, then add 2mL of concentrated sulfuric acid, raise the temperature to about 75°C and reflux for 12h. Cool in an ice-water bath to 0-5°C, add sodium hydroxide solution to adjust the pH to about 8, slowly add 0.10 mol of sodium borohydride solution dropwise, and then raise the temperature to 75°C for 5 hours. Cool in an ice-water bath, adjust the pH value to 5-6 with dilute hydrochloric acid. Recover ethanol under reduced pressure at 40°C, add sodium chloride to the residue until saturated, extract with ethyl acetate, wash the organic layer with saturated brine, and dry over anhydrous sodium sulfate , Ethyl acetate was recovered under reduced pressure to obtain 3,3-dimethylbutanol as a colorless to pale yellow liquid with a yield of 88%.

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PUM

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Abstract

The invention discloses a preparation method of 3,3-dimethyl butanol. According to the preparation method, in ethanol, 3,3-methylbutanoic acid is subjected to esterification under acid catalysis; and one-pot reaction is adopted in the presence of a hydroboron so as to obtain end product 3,3-dimethyl butanol. Using of flammable and combustible reagents (such as lithium aluminium hydride) and solvents (such as ether) is avoided; the end product is obtained via one-pot reaction; yield is high; purity is high; the raw materials are cheap, and source is wide; end product cost is low; and the preparation method is suitable for industrialized production.

Description

technical field [0001] The invention relates to a preparation of 3,3-dimethyl butanol, in particular to a preparation and purification method of 3,3-dimethyl butanol. Background technique [0002] Neotame is a kind of sweetness enhancer discovered in recent times. It was discovered and optimized by the famous NutraSweet company. It is a high-efficiency dipeptide compound, and its chemical name is N-[N-(3,3 -Dimethylbutyl)-L-α-aspartyl]-L-phenylalanine 1-methyl ester, a nitrogen-based derivative of aspartame, which is widely used in food as an enhancer The efficacy of food sweetness. 3,3-Dimethylbutanol is one of the important raw materials for the synthesis of neotame, and the market demand has been increasing in recent years. The traditional method for preparing 3,3-dimethylbutanol is to use 3,3-dimethylbutanoic acid as the starting material, and directly reduce the product with a reducing agent. The commonly used reducing agents are lithium aluminum hydride, sodium boroh...

Claims

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Application Information

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IPC IPC(8): C07C29/147C07C31/125C07C67/08C07C69/24
CPCC07C29/147C07C67/08C07C31/125C07C69/24
Inventor 蒋旭东吕保樱
Owner GUANGXI UNIVERSITY OF TECHNOLOGY
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