Method for synthesis of 2,3-hexanedione monoxime
A technique for the synthesis of hexanedione monoxime, which is applied in oxime preparation, organic chemistry, etc., can solve the problems of low monoxime product yield, and achieve the effects of high reaction yield, easy operation, and fast reaction speed
Inactive Publication Date: 2007-05-16
上海香料研究所
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Problems solved by technology
The yield of the 2,3-hexanedione monoxime product obtained by the usual method is low
Method used
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[0007] The implementation of the present invention will be further described below.
[0008] Into a 500ml round-bottomed three-necked flask equipped with a stirrer, dropping funnel and thermometer, add 130g (1.3mol) of 2-hexanone and 12ml of dilute hydrochloric acid. Under cooling, start to add 200g (1.7mol) of nitrous acid. Isoamyl ester, after dripping, continue to stir for 2 hours, the temperature is always controlled between 40-50 ℃. The reaction yield was 70%. 2,3-Hexanedione monooxime is an important intermediate for the synthesis of 2,3-hexanedione.
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The invention discloses a synthesizing method of 2, 3-acetyl butyryl monooxime, which comprises the following steps: adopting 2-hexanone as raw material; setting the molar rate of 2-hexanone and amyl nitrite at 1: 0.6-1: 0.3; dripping amyl nitrite in the condition of dilute alcaine to react at 20-100 Deg C for 2-10h; making amyl nitrite replace ethyl nitrite.
Description
Technical field [0001] The invention relates to a method for synthesizing 2,3-hexanedione monooxime. Background technique [0002] 2,3-Hexanedione has a strong creamy aroma, sweet creamy aroma; cream and cheese taste, mainly used in soft drinks, baked foods, dairy products and other foods. The 2,3-hexanedione monooxime product obtained by the usual method has a low yield. Summary of the invention [0003] Aiming at the shortcomings of the prior art, the present invention provides a method for synthesizing 2,3-hexanedione monooxime with higher yield. [0004] The synthesis method of 2,3-hexanedione monooxime of the present invention is prepared by using 2-hexanone as a raw material and adding isoamyl nitrite dropwise in the presence of dilute hydrochloric acid. The reaction temperature is 20-100°C, and the reaction time is 2 In -10 hours, the molar ratio of 2-hexanone to isoamyl nitrite is 1:0.6 to 1:3, and the catalyst used in the reaction is dilute hydrochloric acid. The reacti...
Claims
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Login to View More IPC IPC(8): C07C249/04C07C251/38
Inventor 何锡敏黄亚文陶骅
Owner 上海香料研究所