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.), solvent

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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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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