| 第 47 卷第 2 期 |  | Vol. 47 No. 2 | | 2017 年 4 月 | Apr 2017 |
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所屬欄目：農藥及中間體
3-（2-甲基-6-硝基苯基）-4，5-二氫異噁唑的合成研究 |
| 羅先福1，2，3，王曉光1，2，羅和安3，臧陽(yáng)陵1，2，周錦萍1，2，劉國文1，2，黃幼援1，2
（1. 湖南化工研究院有限公司，湖南 長(cháng)沙 410014；2. 農藥化學(xué)品湖南省重點(diǎn)實(shí)驗室，湖南 長(cháng)沙 410014；3. 湘潭大學(xué) 化工學(xué)院，湖南 湘潭 411105） |
| 摘 要：研究了常壓下一鍋法制備 3-（2-甲基-6-硝基苯基）-4，5-二氫異噁唑的方法。原料2-甲基-6-硝基苯甲醛肟溶解后通入氯氣進(jìn)行氯化反應，氮氣吹脫過(guò)量的氯氣和生成的氯化氫后，通入乙烯、滴加縛酸劑進(jìn)行環(huán)合反應得到產(chǎn)品。探索了溶劑、溶劑的量、反應溫度和反應時(shí)間等因素對反應的影響，優(yōu)化條件為以1，2-二氯乙烷為溶劑、溶劑量為原料的5倍、室溫反應、通入乙烯反應8 h，反應轉化率99.5%。優(yōu)化條件下，收率為90.5%。 |
| 關(guān)鍵詞：1，3-偶極環(huán)加成；氯化；2-甲基-6-硝基苯甲醛肟；3-（2-甲基-6-硝基苯基）-4，5-二氫異噁唑 |
| 中圖分類(lèi)號：TQ252.4 文獻標識碼：A 文章編號：1009-9212（2017）02-0032-03 |
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| Synthesis of 3-(2-Methyl-6-nitrophenyl)-4,5-dihydroisoxazole |
| LUO Xian-fu1,2,3, WANG Xiao-guang1,2, LUO He-an3, ZANG Yang-ling1,2, ZHOU Jin-ping1,2, LIU Guo-wen1,2, HUANG You-yuan1,2
(1. National Engineering Center for Agrochemicals, Hunan Research Institute of Chemical Industry Co., Ltd., Changsha 410014, China; 2. Hunan Province Key Laboratory for Agrochemicals, Changsha 410014, China; 3. College of Chemical Engineering, Xiangtan University, Xiangtan 411105, China) |
| Abstract：One-pot synthesis of 3-(2-methyl-6-nitrophenyl)-4,5-dihydroisoxazole under atmospheric pressure was studied. Chlorine was induced to the solution of 2-methyl-6-nitrobenzaldehyde oxime. After the chlorination process was completed, nitrogen was induced to blow off the excess chlorine and the generated hydrogen chloride. Then ethylene was introduced and the acid binding agent was added. The product was synthesized by 1,3-dipolar cycloaddition. The effects of solvent, reaction temperature and time on the reaction were explored. Optimal conditions were as followings: 1,2-dichloroethane as solvent, the amount of solvent as 5 times quality of the raw materials, room temperature reaction and ethylene reaction for 8 hours, the reaction conversion rate of 99.5% was obtained and the yield was up to 90.5%. |
| Key words：1,3-dipolar cycloaddition; chlorination; 2-methyl-6-nitrobenzaldehyde oxime; 3-(2-methyl-6-nitrophenyl)-4,5-dihydroisoxazole |
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基金項目：國家自然科學(xué)基金（21672057）。
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作者簡(jiǎn)介：羅先福（1983-），男，湖南津市人，博士，助理研究員，主要從事藥物及其中間體的綠色合成工藝研究（E-mail：luofu1109@163.com）
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收稿日期：2017-02-18
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