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Method for synthesizing high-recovery and high-optical purity L-butyl lactate

A technology for butyl lactate and synthesis methods, applied in chemical instruments and methods, preparation of carboxylic acid esters, organic chemistry, etc., can solve the problem of high cost and achieve the effect of avoiding losses

Inactive Publication Date: 2003-10-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these catalysts only need to be filtered after the reaction, the production process can be simplified, but the cost is higher than that of sulfuric acid (the price of sulfuric acid is 280 yuan / ton, the price of p-toluenesulfonic acid is 2800 yuan / ton, and the price of ferric chloride is 3500 yuan / ton )

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0008] Add 480g of lactic acid, 348g of benzene, 640g of n-butanol and 7.36g of concentrated sulfuric acid into a 2000ml reaction flask equipped with a water separator and a reflux condenser, reflux at 80-100°C for 17 hours, and divide 156ml of water. Directly add 11.93g solid anhydrous sodium carbonate to neutralize sulfuric acid after the reaction finishes, the mol ratio of solid anhydrous sodium carbonate and concentrated sulfuric acid is 1.5: 1, then filter. The yield of L-butyl lactate was 90%, and the optical purity was 99.5%.

example 2

[0010] Add 480g of lactic acid, 348g of benzene, 505g of n-butanol and 7.36g of concentrated sulfuric acid into a 2000ml reaction flask equipped with a water separator and a reflux condenser, reflux at 80-100°C for 17 hours, and divide 156ml of water. Directly add 14.32g solid anhydrous sodium carbonate to neutralize sulfuric acid after the reaction finishes, the mol ratio of solid anhydrous sodium carbonate and the concentrated sulfuric acid is 1.8: 1, then filter. The yield of L-butyl lactate was 90%, and the optical purity was 99.7%.

example 3

[0012] Add 480g of lactic acid, 348g of benzene, 370g of n-butanol and 7.36g of concentrated sulfuric acid into a 2000ml reaction flask equipped with a water separator and a reflux condenser, reflux at 80-100°C for 17 hours, and divide 156ml of water. Directly add 15.91g solid anhydrous sodium carbonate to neutralize sulfuric acid after the reaction finishes, the molar ratio of solid anhydrous sodium carbonate and concentrated sulfuric acid is 2: 1, then filter. The yield of L-butyl lactate was 91%, and the optical purity was 99.8%.

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Abstract

The method for synthesizing L-butyl lactate with high yield and high optical purity uses concentrated sulfuric acid as catalyst, the added quantity of the concentrated sulfuric acid is 1.5% of lacticacid mass, the mole ratio of the n-butyl alcohol and lactic acid can be 0.5-4, reaction temp. is 50-150 deg.c, after the reaction is completed the solid anhydrous sodium acetate, solid anhydrous sodium carbonate, solid anhydrous sodium hydroxide or solid anhydrous sodium hydroxide can be directly added to neutralize sulfuric acid, then the above-mentioned material is filtered and separated so as to obtain the invented product. Its yield rate is up to above 90% and its optical purity is up to above 99.5%.

Description

technical field [0001] The present invention relates to the synthesis method of L-butyl lactate, especially in the process of synthesizing L-butyl lactate and the post-treatment process, reducing the loss of L-butyl lactate, avoiding racemization, and improving the L-butyl lactate Optical purity and yield of esters. Background technique [0002] Butyl lactate is an important class of α-hydroxy ester compounds. It is a colorless, stable, mild-smelling, slightly water-soluble liquid. At the same time, it is a high boiling point solvent with excellent performance and wide application, mainly used in natural resins, synthetic resins, paints, printing inks, dry cleaning fluids, adhesives, etc. It is also a popular edible synthetic spice. It can be used in some soft drinks, ice cream and other foods. Especially the optically active L-butyl lactate can be used as an intermediate of green pesticides. At present, concentrated sulfuric acid is used as a catalyst in the industrial ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/68
Inventor 刘菁李德才徐杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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