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Process for synthesizing milk lactone

A technology of milk lactone and synthesis process, applied in the field of food additives, can solve the problems of high cost, complicated operation, harsh reaction conditions and the like, and achieve the effect of improving yield

Inactive Publication Date: 2014-06-18
GUANGDONG GUANGYI TECH IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Chinese patent CN1266841A uses n-butyraldehyde and cyclohexanone as raw materials, undergoes alkaline condensation, selective hydrogenation, ring expansion of hydrogen peroxide to lactone, and finally dehydration under acidic conditions to obtain 5(6)-decenoic acid. When the reaction is alkaline condensation, the reaction is slow, and the reaction yield is low, and the separation and purification process is cumbersome, resulting in the disadvantages of high cost, harsh reaction conditions, complicated operation, and low yield in the entire synthesis route.

Method used

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  • Process for synthesizing milk lactone
  • Process for synthesizing milk lactone
  • Process for synthesizing milk lactone

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The synthetic technique of milk lactone, it specifically comprises the following steps:

[0029] 1. Synthesis of 2-butylene cyclohexanone

[0030] In a 500mL three-neck flask equipped with a thermometer, a stirrer, and a dropping funnel, add 180mL of 1% sodium hydroxide solution, 5.40g of polyethylene glycol 400, 176.67g (about 1.8mol) of cyclohexanone, After mixing the above materials evenly, add 86.52 g (about 1.2 mol) of n-butyraldehyde into the three-necked flask dropwise through the dropping funnel, and stir while dropping. After 1 hour, the dropwise addition is completed, and then continue to stir, so that the above reactants are heated at 30 ° C. Under reaction 2h.

[0031] After the reaction, add about 6mL of glacial acetic acid into the three-necked flask, neutralize the water layer to a pH of 6-7, and then separate the oil layer after standing for a while; extract the water layer with 300mL of toluene , and the extracted toluene solution and the oil layer we...

Embodiment 2

[0042]The synthetic technique of milk lactone, it specifically comprises the following steps:

[0043] 1. Synthesis of 2-butylene cyclohexanone

[0044] The difference between this step and Example 1 is that the phase-transfer catalyst used is different, and the phase-transfer catalyst used in this embodiment is cetyltrimethylammonium chloride;

[0045] In a 500mL three-necked flask equipped with a thermometer, a stirrer, and a dropping funnel, add 200mL of 1% sodium hydroxide solution, 5.00g of cetyltrimethylammonium chloride, 196.28g (about 2.0mol ) cyclohexanone, after the above materials are mixed evenly, then dropwise add 86.52g (about 1.2mol) of n-butyraldehyde in the three-necked flask through the dropping funnel, stir while dripping, 1h dropwise, continue to stir subsequently, make the above The reactants were reacted at 30°C for 2h.

[0046] After the reaction, add about 6mL of glacial acetic acid into the three-necked flask, neutralize the water layer to a pH of 6-...

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Abstract

The invention relates to the technical field of a feed additive, and particularly relates to a flavoring matter with milk fragrance, namely milk lactone, also named a 5(6)-caproleic acid. The invention provides a novel process for preparing milk lactone. The process comprises the following steps: carrying out alkaline condensation under the action of a phase-transfer catalyst by taking n-butanal and cyclohexanone as raw materials; carrying out catalytic hydrogenation to obtain 2-butyl-cyclohexanone after dewatering; oxidizing the 2-butyl-cyclohexanone to obtain epsilon-decalactone by a superoxide; and directly hydrolyzing and dewatering the epsilon-decalactone to obtain the 5(6)-caproleic acid. The process is available in raw material, simple to operate, low in cost and relatively high in productivity.

Description

technical field [0001] The invention relates to the technical field of food additives, in particular to a synthesis process of milk lactone. Background technique [0002] Milk lactone is a mixture of 5(6)-decenoic acids, English name: 5(6)-decenoic acids mixture, is a food additive with milk flavor. It is actually a kind of unsaturated fatty acid. This very small amount of unsaturated fatty acid can produce milk flavor, strong aroma and long-lasting fragrance. It is a safe edible flavor approved by the American Practical Flavor Manufacturers Association. , cream, cheese essence, chocolate and other important raw materials of food. In addition, milk lactone has a high boiling point and can be used in baked foods. It is not easily destroyed like the compound milk flavor, and its application prospect is very broad. [0003] Chinese patent CN1266841A uses n-butyraldehyde and cyclohexanone as raw materials, undergoes alkaline condensation, selective hydrogenation, ring expansio...

Claims

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Application Information

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IPC IPC(8): C07C57/03C07C51/377
CPCC07C45/62C07C45/74C07C51/09C07C51/377C07C2601/14C07D313/04C07C57/03C07C59/01C07C49/603C07C49/403
Inventor 王立武
Owner GUANGDONG GUANGYI TECH IND
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