第 42 卷第 3 期 |  | Vol. 42 No. 3 | 2012 年 6 月 | Jun 2012 |
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所屬欄目:醫藥及中間體
5-溴代胡椒環(huán)的合成方法研究 |
姜 輝,趙素娟,趙 巍,王海波,王海洋*,王守凱
(中鋼集團鞍山熱能研究院有限公司,遼寧 鞍山 114044) |
摘 要:以胡椒環(huán)為原料,采用氧化溴化體系合成5-溴代胡椒環(huán),確定了溴化工藝條件,考察了溶劑種類(lèi)、反應溫度、物料配比及反應時(shí)間對反應的影響。優(yōu)化工藝為:三氯甲烷為反應溶劑,反應溫度為10℃,反應時(shí)間為6 h,物料配比n(胡椒環(huán)) ∶n(氫溴酸)=1∶1.2。產(chǎn)品收率 81%,產(chǎn)品純度99.5%(GC)。產(chǎn)物的結構經(jīng)1H NMR、IR、MS表征。 |
關(guān)鍵詞:溴代胡椒環(huán);溴化;合成 |
中圖分類(lèi)號:TQ0625.21 文獻標識碼:A 文章編號:1009-9212(2012)03-0047-03 |
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Study on Synthesis of 5-Bromo-pepper Ring |
JIANG Hui,ZHAO Su-juan,ZHAO Wei,WANG Hai-bo,WANG Hai-yang,WANG Shou-kai
(Sinosteel Anshan Research Institute of Thermo-Energy Co.,Ltd. Anshan 114044,China) |
Abstract:5-Bromo-pepper ring was synthesized from pepper ring by its bromination with H2O2/HBr or bromine. The reaction conditions of the H2O2/HBr system were investigated. The optimum conditions were as followings:chloroform as the reaction solvent,reaction temperature of 10℃,reaction time of 6 hours,molar ratio of pepper ring to hydrogen bromide of 1.0∶1.2. The target product was obtained in 81% yield(purity 99.5% GC)and its structure was confirmed with IR,1H NMR and MS. |
Key words:5-bromo-pepper ring;bromination;synthesis |
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作者簡(jiǎn)介:姜 輝(1981-),男,遼寧鞍山人,工程師,碩士,主要從事精細化工中間體及煤焦油深加工研究。(E-mail:jianghui5168@126.com)
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聯(lián) 系 人:王海洋,工程師。主要從事精細化工。(E-mail:haiyangwang2008@yahoo.com.cn)
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收稿日期:2012-02-13
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