第 45 卷第 1 期 |  | Vol. 45 No. 1 | 2015 年 2 月 | Feb 2015 |
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所屬欄目:醫藥及中間體
3,5-二氯-2-戊酮的合成研究 |
陳明明1,2,3,劉 偉2,3,5,陳蒙慈4,曾雪云2,3,陳 明2,3 *
(1. 湖南師范大學(xué) 化學(xué)化工學(xué)院,湖南 長(cháng)沙 410081;2. 湖南化工研究院 國家農藥創(chuàng )制工程技術(shù)研究中心,湖南 長(cháng)沙 410014;3. 農用化學(xué)品湖南省重點(diǎn)實(shí)驗室,湖南 長(cháng)沙 410014;4. 湖南海利化工股份有限公司,湖南 長(cháng)沙 410007;5. 湖南大學(xué) 化學(xué)化工學(xué)院,湖南 長(cháng)沙 410082) |
摘 要:以α-氯-α-乙;-γ-丁內酯、固體光氣為原料,N,N-二甲基哌啶鹽酸鹽為催化劑合成了3,5-二氯-2-戊酮?疾炝舜呋瘎┓N類(lèi)、氮氣通入速率、物料配比、滴加時(shí)間、滴加溫度等因素對反應的影響。優(yōu)化條件下,3,5-二氯-2-戊酮的含量94.0%,收率81.5%(以α-氯-α-乙;-γ-丁內酯計)。 |
關(guān)鍵詞:α-氯-α-乙;-γ-丁內酯;固體光氣;N,N-二甲基哌啶鹽酸鹽;3,5-二氯-2-戊酮;合成 |
中圖分類(lèi)號:TQ215 文獻標識碼:A 文章編號:1009-9212(2015)01-0036-03 |
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Synthesis of 3,5-Dichloro-2-Pentanone |
CHEN Ming-ming1,2,3, LIU Wei2,3,5, CHEN Meng-ci4, ZENG Xueyun2,3, CHEN Ming2,3
(1. Department of Chemistry and Chemical Engineering, Hunan Normal University, Changsha 410081; 2. Hunan Research Institute of Chemical Industry, Changsha 410014, China; 3. Hunan Province Key Laboratory for Agrochemicals, Changsha 410014, China; 4. Hunan Haili Chemical Industrial Co., Ltd., Changsha 410007, China; 5. Institute of Chemistry and Chemical Engineering, Hunan University, Changsha 410082, China) |
Abstract:The synthesis of 3,5-dichloro-2-pentanone was achieved with α-acetyl-α-chloride-γ-butyrolactone and triphosgene as raw materials, and N,N-dimethyl-piperidine hydro-chloride as the catalyst. The main influence factors including temperature, the dropping time of triphosgene, the ratio of materials, the types of catalysts, the blowing rate of nitrogen and other factors were evaluated. Under the best condition of reaction, the purity of 3,5-dichloro-2-pentanone reached 94.0%, and the yield was up to 81.5% based on the starting material of α-acetyl-α-chloride-γ-butyrolactone. |
Key words:α-acetyl-α-chloride-γ-butyrolactone; bis(trichloromethyl)carbonate; N,N-dimethyl-piperidine hydrochloride; 3,5-dichloro-2-pentanone |
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作者簡(jiǎn)介:陳明明(1988-),男,河南淮陽(yáng)人,碩士研究生,主要從事化學(xué)工程與工藝研究。
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聯(lián) 系 人: 陳 明,研究員,主要從事農藥及中間體研究(E-mail:chegming1@163.com)。
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收稿日期:2015-01-10
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