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Synthetic method of 2,3-heptane dione

A technology of heptanedione and heptanedione monoxime, which is applied in the preparation of carbonyl compounds by hydrolysis and organic chemistry, can solve the problems of slow reaction speed, complicated operation and low reaction yield, and achieve fast reaction speed and high reaction yield. High, easy-to-handle effects

Inactive Publication Date: 2009-05-06
上海香料研究所
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AI Technical Summary

Problems solved by technology

The current synthetic method of 2,3-heptanedione is complex in operation, slow in reaction speed and low in reaction yield

Method used

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  • Synthetic method of 2,3-heptane dione

Examples

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Embodiment Construction

[0007] The following examples further illustrate the present invention.

[0008] Into a 500ml round-bottomed three-necked flask equipped with a stirrer, dropping funnel and thermometer, add 150g (1.3mol) of 2-heptanone and 12ml of dilute hydrochloric acid, and start to add 200g (1.7mol) of nitrous acid dropwise under cooling. Isoamyl ester, after dripping, continue to stir for 2 hours, the temperature is always controlled between 40-50 ℃. The reaction yield was 71.8%.

[0009] Add the 2,3-heptanedione monooxime prepared above and 2210 ml of water into a 5000 ml three-necked flask, and add a mixture of 180 g of sodium nitrite and 450 ml of water, heat and stir to 45°C, and then add 600 ml dropwise. G 30% dilute sulfuric acid solution, drip in about 1 hour. Stirring is continued for 4 hours, maintaining the reaction temperature between 50 and 60°C. Use 5% Na 2 CO 3 Solution washing, anhydrous MgSO 4 After drying, 138 grams of crude 2,3-heptanedione (content 74%) was obtained. The cr...

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Abstract

The invention discloses a method for synthesizing 2, 3-heptanedione, which comprises the following steps: 2, 3-heptanedione monoxime is prepared by taking 2-heptanone as a raw material and dripping isoamyl nitrite in the presence of dilute hydrochloric acid, and then performing hydrolysis. The hydrolysis temperature is between 20 and 60 DEG C, the hydrolysis time is between 4 and 10 hours, and a catalyst for the hydrolysis is the dilute hydrochloric acid. The method has easy operation, quick reaction rate, and high reaction yield.

Description

Technical field [0001] The present invention relates to a synthesis method of 2,3-heptanedione. Background technique [0002] 2,3-Heptanedione has a strong oily aroma, a cheese-like spicy smell and a sweet creamy taste. It is mainly used in soft drinks, baked foods, dairy products, chewing gum and other foods. At present, the synthesis method of 2,3-heptanedione is complicated, the reaction speed is slow, and the reaction yield is low. Summary of the invention [0003] In view of the above-mentioned problems, the present invention provides a method for synthesizing 2,3-heptanedione that is easy to operate, fast in reaction speed, and high in reaction yield. [0004] The method for synthesizing 2,3-heptanedione of the present invention: Take 2-heptanone as a raw material, add isoamyl nitrite dropwise in the presence of dilute hydrochloric acid to prepare 2,3-heptanedione monooxime, and then mix 2, 3-Heptanedione monooxime can be hydrolyzed. The reaction formula is as follows: [...

Claims

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Application Information

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IPC IPC(8): C07C49/12C07C45/43
Inventor 何锡敏黄亚文陶骅郦云临
Owner 上海香料研究所
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