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Production of unsaturated ketone

An unsaturated, alkoxypropylene technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of carbon-based compounds, etc., can solve the problems of using volatile organic solvents, catalysts cannot be recycled, and simplify the separation process. , easy to operate, simple reaction process

Active Publication Date: 2006-08-16
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a green method for preparing unsaturated ketones, which solves the defects in the prior art, such as catalysts that cannot be recycled, use of volatile organic solvents, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Dehydrolinalool (0.15mol) and [Bmim][HSO 4 ] (0.0015mol) was added to a 250ml three-necked flask, and the three-necked flask was placed in an oil bath, heated to 100°C under stirring, and at the same time, 2-ethoxypropylene (0.375mol) was added dropwise, and after 24 hours of reaction , add water to cool and stir to mix, and separate the product and the liquid phase. The organic phase is evaporated to remove the low-boiling components, which is the product with a yield of 90% and a content of 97%.

Embodiment 2

[0024] Dehydrolinalool (0.15mol) and [Et 3 NH][HSO 4 ] (0.0015mol) was added to a 250ml three-necked flask, and the three-necked flask was placed in an oil bath, heated to 100°C under stirring, and at the same time, 2-ethoxypropylene (0.375mol) was added dropwise, and after 24 hours of reaction , add water to cool and stir to mix, and separate the product and the liquid phase. The organic phase is evaporated to remove the low-boiling components to obtain the product with a yield of 93% and a content of 98%.

Embodiment 3-12

[0026] Similar to Example 1, use [Emim][HSO 4 ], [Hmim][HSO 4 ], [Bmim][H 2 PO 4 ], [Me 3 NH][HSO 4 ], [Me 3 NH][H 2 PO 4 ] as solvent and catalyzer, react under different conditions, obtain following result (table one) after finishing:

[0027] Reality

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PUM

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Abstract

Production of unsaturated ketone is carried out by taking unsaturated alcohol and 2-alkoxy-propene as raw materials, taking acid ion as catalyst and reactive solvent, Saucy-Marbet reacting and synthesizing unsaturated ketone. It has better selectivity and recovery rate, non-volatility and no environmental pollution.

Description

technical field [0001] The invention relates to a new method for preparing unsaturated ketones. The method uses unsaturated alcohol as a starting material, and uses an environmentally friendly acidic ionic liquid as a catalyst and a reaction solvent under the condition of no volatile organic solvent and catalyst. Saucy-Marbet reaction with 2-alkoxypropene can produce unsaturated ketone with high yield and high selectivity. Background technique [0002] Unsaturated ketones are important intermediates for the synthesis of spices, essences, vitamins, and medicines. For example, methyl heptenone, also known as 5-methyl-3-hepten-2 ketone, is an important raw material for the synthesis of perfume and pharmaceutical intermediate linalool; pseudoionone, also known as 6,10-dimethyl -3,5,9-Tridecen-2-one, molecular formula C 13 h 20 O is an important raw material for the synthesis of ionone, vitamin A, β-carotene, etc., and is widely used in the perfume and pharmaceutical industrie...

Claims

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Application Information

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IPC IPC(8): C07C45/00C07C49/20B01J31/02
Inventor 李浩然王从敏王勇郭丽萍胡柏剡
Owner ZHEJIANG UNIV
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