第 51 卷第 2 期 |  | Vol. 51 No. 2 | 2021 年 4 月 | Apr 2021 |
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所屬欄目:農藥及中間體
呋喃磺草酮關(guān)鍵中間體的合成工藝研究 |
張小涵,王 寧,袁美嬌,黃朋勉*
(長(cháng)沙理工大學(xué) 化學(xué)與食品工程學(xué)院,湖南 長(cháng)沙 410000) |
摘 要:以2-氯-4-甲硫基-3-甲基苯乙酮(3)為原料,在鎢酸鈉催化條件下,經(jīng)過(guò)氧化氫氧化得到2-氯-4-甲磺;-3-甲基苯乙酮(2),優(yōu)化條件下收率達98.31%。2 與次氯酸鈉進(jìn)行氯仿反應得到2-氯-4-甲磺;-3-甲基苯甲酸(1),優(yōu)化條件下收率達95.25%。兩步收率93.64%;衔1、2、3均經(jīng)氫譜確認結構。該制備方法清潔高效、收率較高、成本較低,工業(yè)化生產(chǎn)前景廣闊。 |
關(guān)鍵詞:2-氯-4-甲硫基-3-甲基苯乙酮;2-氯-4-甲磺;-3-甲基苯乙酮;2-氯-4-甲磺;-3-甲基苯甲酸 |
中圖分類(lèi)號:TQ463 文獻標識碼:A 文章編號:1009-9212(2021)02-0029-03 |
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Synthesis of Key Intermediate of Furansulfoxanone |
ZHANG Xiao-han, WANG Ning, YUAN Mei-jiao, HUANG Peng-mian*
(Changsha University of Science and Technology, College of Chemical and Food Engineering, Changsha 410000, China) |
Abstract:Using 2-chloro-4-methyl-3-methylacetophenone (3) as the raw material, 2-chloro-4-methosulfonyl-3-methylacetophenone(2) was synthesized by hydrogen peroxide catalyzed by sodium tungstate with a yield of 98.31% for 2-chloro-4-methylsulfonyl-3-methylacetophenone (2) under optimized conditions. Chloroform reaction of 2 with sodium hypochlorite was carried out to obtain 2-chloro-4-methosulfonyl-3-methylbenzoic acid (1), and the yield reached 95.25% under optimized conditions. The final total yield could reach up to 93.64%. Substances 1, 2 and 3 were characterized by 1H NMR. This preparation method was green and efficient with high yield and low cost, and has broad prospects for industrial production. |
Key words:2-chloro-4-methyl-3-methylacetophenone; 2-chloro-4-methosulfonyl-3-methylacetophenone; 2-chloro-4-methosulfonyl-3-ethylbenzoic acid |
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基金項目:湖南省教育廳科學(xué)研究項目(20A019)。
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作者簡(jiǎn)介:張小涵(2000—),女,湖南常德人,研究方向:有機合成(E-mail:2665913677@qq.com)。
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聯(lián) 系 人:黃朋勉,副教授,研究方向:有機合成(E-mail:280897806@qq.com)。
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收稿日期:2021-04-02
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