Phosphite Ester Catalyzed Synthesis of Gamma-Delta-Unsaturated Ketones

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

Current methods for manufacturing gamma, delta-unsaturated ketones are not sustainable and efficient, particularly in producing specific compounds like 6-methyl-5-hepten-2-one, 6-methyl-5-octen-2-one, and their derivatives, as they rely on less effective catalysts such as phosphonic acids or ammonium salts.

Innovation Solution

A process using novel catalysts like diphenyl phosphite, dimethyl phosphite, and dibenzyl phosphite to react tertiary vinyl carbinols with isopropenyl alkyl ethers at specific molar ratios, temperatures, and pressures to produce gamma, delta-unsaturated ketones, optimizing the reaction conditions for high conversion and selectivity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If phosphonic acids or ammonium salts are used as catalysts, then the manufacturing process can be established, but the sustainability and efficiency are insufficient

Engineering Contradiction:
ImprovesustainabilityVSAvoidefficiency
Core Design Contradiction:
ReliabilityVSProductivity

Solution Approach 1:

The patent changes the chemical parameter of the catalyst from phosphonic acids or ammonium salts to phosphite esters (specifically diphenyl phosphite, dimethyl phosphite, or dibenzyl phosphite). This parameter change in catalyst structure and composition resolves the contradiction by providing both improved sustainability through better environmental profile and enhanced efficiency through superior catalytic activity and selectivity for gamma,delta-unsaturated ketone production

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If conventional catalysts are used, then the process can proceed, but conversion and selectivity are not optimized

Engineering Contradiction:
ImproveselectivityVSAvoidconversion
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent optimizes the catalyst parameter by selecting specific phosphite esters (diphenyl phosphite, dimethyl phosphite, or dibenzyl phosphite) which provide both high selectivity for the desired gamma,delta-unsaturated ketone product and high conversion of starting materials. The catalyst amount is also optimized at 0.01-0.30 mol% based on the tertiary vinyl carbinol, achieving simultaneous improvement in both selectivity and conversion

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs a composite approach by combining specific phosphite ester catalysts with controlled reaction conditions (temperature 100-170°C, pressure 5-15 bar, molar ratio 1:7 to 1:1) to create an optimized catalytic system that achieves both high conversion and high selectivity, overcoming the limitations of conventional single-parameter optimization

Inventive Principle:
Principle #40Composite materials

3Manufacturing precision

If the reaction conditions are not optimized, then the process is simpler, but conversion and selectivity suffer

Engineering Contradiction:
ImproveconversionVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent establishes optimized parameter ranges for the reaction process: temperature 100-170°C, pressure 5-15 bar, and molar ratio of tertiary vinyl carbinol to isopropenyl alkyl ether from 1:7 to 1:1. These parameter changes achieve high conversion and selectivity while maintaining reasonable process complexity through defined operational windows

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 conversion and selectivity in producing gamma, delta-unsaturated ketones, such as 6-methyl-5-hepten-2-one and its derivatives, with preferred catalysts like DPPI, DMPI, and DBPI, offering an industrial-scale, sustainable solution.

Implementation Method 1

reacting a tertiary vinyl carbinol of the general formula (I) with an isopropenyl alkyl ether of the general formula (II) in the presence of a catalyst of the general formula (IV)

Methodology Applied
Scientific EffectCatalysis: Catalysis

Data Source

PatentEP3541775B1Novel process for the manufacture of gamma,delta-unsaturated ketones
Publication Date: 2022.07.27 DSM IP ASSETS BV
  • EP3541775B1 patent drawingFigure 1~4
  • EP3541775B1 patent drawingFigure 5~6
  • EP3541775B1 patent drawing

AI summary

The present invention is directed towards an industrial sustainable process for the manufacture of gamma, delta-unsaturated ketones of formula (III ) in the presence of novel catalysts of formula (IV), wherein R1 is methyl or ethyl, R3 is methyl, R2 is a saturated or unsaturated linear, branched or cyclic hydrocarbyl group with 1 to 46 C atoms, and R and R' are independently from each other selected from the group consisting of linear C1-6-alkyl, branched C3-6-alkyl, aryl and aralkyl (see also Fig.1). The present invention is especially directed towards an industrial sustainable process for the manufacture of 6-methyl-5-hepten-2-one ("MH"; see Fig. 2), 6-methyl-5-octen-2-one ("EH"; see Fig. 3), (5EZ)-6, 10-dimethyl- 5,9-undecadien-2-one (f)-geranylacetone = "GA"; (Z)-nerylacetone = "NA"; see Fig. 4), (5fZ)-6, 10-dimethyl-5-undecen-2-one ((f)-dihydrogeranyl- acetone = "DHGA"; (Z)-dihydronerylacetone = "DHNA"; see Fig. 5) and 6, 10, 14-trimethyl-5,9, 13-pentadeca-trien-2-one (= farnesylacetone; "FA"; see Fig. 6). Preferred catalysts according to the present invention are "DPPI" (diphenyl phosphite), "DMPI" (dimethyl phosphite) and "DBPI" (dibenzyl phosphite).