Aqueous Lactam Ring-Opening for Amino Acid Ester Synthesis

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Solution Overview

Problem

Current methods for synthesizing organosulfate salts of amino acid esters require handling of organic solvents and corrosive acids, are complex, and have low yields with long reaction times, and struggle with reacting amino acids and lactams with low water solubility alcohols.

Innovation Solution

A process involving the reaction of lactams with sulfuric acid in an aqueous solution, followed by esterification with excess alcohol in water, allowing for the synthesis of organosulfate salts of amino acid esters without organic solvents and corrosive acids, using a single reaction step with high yield and reduced complexity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If current methods are used for synthesizing organosulfate salts of amino acid esters, then the synthesis can be performed with existing processes, but handling of organic solvents and corrosive acids is required, and yields are low with long reaction times

Engineering Contradiction:
Improvereaction timeVSAvoidhandling of organic solvents and corrosive acids
Core Design Contradiction:
ProductivityVSObject-affected harmful factors

Solution Approach 1:

The invention changes the reaction medium from organic solvents to water as the solvent system, and modifies the acid form from corrosive concentrated acids to milder acid forms, thereby eliminating harmful handling while maintaining reaction efficiency and improving productivity

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention uses water as a disposable, non-toxic solvent that can be easily removed, replacing expensive and hazardous organic solvents that require special handling and disposal procedures

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

2Ease of manufacture

If current methods are used for synthesizing organosulfate salts of amino acid esters, then existing synthesis routes can be followed, but the processes are complex with multiple steps

Engineering Contradiction:
Improveprocess complexityVSAvoidsynthesis efficiency
Core Design Contradiction:
Ease of manufactureVSProductivity

Solution Approach 1:

The invention combines multiple separate synthesis steps into a single one-pot reaction where amino acid ester and organosulfate are formed simultaneously in water, eliminating the need for separate organic solvent steps and simplifying the overall manufacturing process

Inventive Principle:
Principle #5Merging (Combining)

3Manufacturing precision

If current methods are used for synthesizing organosulfate salts of amino acid esters, then traditional esterification can be performed, but yields are low

Engineering Contradiction:
Improvesynthesis yieldVSAvoidreaction time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The invention changes the esterification conditions by performing the reaction in water with specific pH control and temperature parameters, which dramatically improves the yield of organosulfate salt formation while reducing the time required to reach completion

Inventive Principle:
Principle #35Parameter changes

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This process achieves high yield and fast reaction times, eliminating the need for organic solvents and corrosive acids, and effectively synthesizes organosulfate salts of amino acid esters, suitable for detergent formulations.

Implementation Method 1

the ring -opening of the lactam to obtain the amino acid in presence of an acid

Methodology Applied
Scientific EffectRing-opening reaction: Chemical Bonding

Implementation Method 2

as a second step the esterification reaction with an alcohol

Methodology Applied
Scientific EffectEsterification reaction: Chemical Bonding

Implementation Method 3

TRIVEDI, T. J. et al. ChemSusChem 2011, number 4, pages 604-608 describe a synthesis route to salts from alpha- C 3 -C 4 -amino acid esters and laurylsulfate

Methodology Applied
Scientific EffectSalt formation reaction: Chemical Bonding

Data Source

PatentEP3908572B1Process for the preparation of organosulfate salts of amino acids esters
Publication Date: 2024.06.19 BASF SE

AI summary

The present invention relates to a process for the synthesis of organosulfate salts of amino acid esters comprising the steps of reacting at least one lactam with at least 3 carbon atoms in the lactam ring with sulfuric acidin an aqueous solution followed by esterification of the reaction product of the previous step with at least 200 mol-% of at least one alcohol selected from the group consisting of linear alkyl alcohol containing one hydroxy group, branched alkyl alcohol containing one hydroxy group, linear alkylether alcohol containing one hydroxy group, branched alkylether alcohol containing one hydroxy group, phenoxyalkanols containing one hydroxy group, and mixtures thereof; followed optionally removal of water and/or removal of excess alcohol.