| 第 51 卷第 5 期 |  | Vol. 51 No. 5 | | 2021 年 10 月 | Oct 2021 |
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所屬欄目：農藥及中間體
中間體3，5-二氯-2-戊酮的綠色合成工藝開(kāi)發(fā) |
| 丁亞偉1，張紹勇2，楊丙連1*
（1. 上海泰禾化工有限公司，上海 201612；2. 湖州師范學(xué)院，浙江省媒介生物學(xué)與病原控制重點(diǎn)實(shí)驗室，浙江 湖州 313000） |
| 摘 要：α-乙�；�-γ-丁內酯與氯氣在無(wú)溶劑條件下發(fā)生氯化反應，得到α-氯-α-乙�；�-γ-丁內酯和副產(chǎn)氯化氫，α-氯-α-乙�；�-γ-丁內酯在少量水和氯化氫的存在下進(jìn)行開(kāi)環(huán)、氯代和脫羧反應得到3,5-二氯-2-戊酮。對氯氣投料比、反應溫度、氯化氫用量等因素進(jìn)行優(yōu)化。優(yōu)化工藝條件為，第一步反應：氯化溫度為0~5 ℃、n（氯氣）∶n（α-乙�；�-γ-丁內酯）=1.07∶1.00；第二步反應：水解、脫羧及氯化溫度為90 ℃、n（氯化氫）∶n（α-氯-α-乙�；�-γ-丁內酯）=0.7∶1.0，n（水）∶n（α-氯-α-乙�；�-γ-丁內酯）=0.8∶1.0，通入氯化氫4 h，此條件下，收率達95.2%。 |
| 關(guān)鍵詞：α-乙�；�-γ-丁內酯；α-氯-α-乙�；�-γ-丁內酯；3，5-二氯-2-戊酮 |
| 中圖分類(lèi)號：S482.2 文獻標識碼：A 文章編號：1009-9212（2021）05-0027-04 |
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| Synthesis of 3,5-Dichloro-2-pentanone |
| DING Ya-wei1, ZHANG Shao-yong2, YANG Bing-lian1*
(1. R&D Center of CAC Shanghai International Trading Co.,Ltd., Shanghai 201612, China; 2. Key Laboratory of Vector Biology and Pathogen Control of Zhejiang Province, College of Life Sciences, Huzhou University, Huzhou 313000, China) |
| Abstract：The reaction between α-acetyl-γ-butyrolactone and chlorine gas under solvent-free conditions gives α-chloro-α-acetyl-γ-butyrolactone and the by-product hydrogen chloride. Then, α-chloro-α-acetyl-γ-butyrolactone undergoes ring opening reaction and decarboxylation reactions in the presence of a small amount of water and hydrogen chloride to obtain 3,5-dichloro-2-pentanone. The reaction conditions including chlorine feed ratio, reaction temperature, hydrogen chloride dosage and other factors were optimized. The optimized process conditions were as followings: the chlorination temperature was in a range from 0 ℃ to 5 ℃; the amount of chlorine gas was 1.07 times of α-chloro-α-acetyl-γ-butyrolactone in molar mass; the temperature of hydrolysis, decarboxylation and chlorination was of 90 ℃; the amount of hydrogen chloride was 0.7 times of α-chloro-α-acetyl-γ-butyrolactone in molar mass; the amount of water was 0.8 times of α-chloro-α-acetyl-γ-butyrolactone in molar mass; and the yield was 95.2%. |
| Key words：α-acetyl-γ-butyrolactone; α-chloro-α-acetyl-γ-butyrolactone; 3,5-dichloro-2-pentanone |
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作者簡(jiǎn)介：丁亞偉（1985—），男，河南夏邑人，工程師，主要從事農藥及中間體合成研究（E-mail：yawei.ding@163.com）。
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聯(lián) 系 人：楊丙連，高級工程師，主要從事農藥及中間體合成研究（E-mial：bingliany@126.com）。
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收稿日期：2021-08-03
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