第 37 卷第 5 期 |  | Vol. 37 No. 5 | 2007 年 10 月 | Oct 2007 |
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所屬欄目:醫藥及中間體
催化加氫制備萘丁美酮工藝研究 |
李巍巍1,2,童國通1,呂路平1
(1.杭州職業(yè)技術(shù)學(xué)院 化工系,浙江 杭州 310018;2.浙江工業(yè)大學(xué) 化學(xué)工程與材料學(xué)院,浙江 杭州 310014) |
摘 要:選取催化劑、溶劑、脫水劑、溫度、壓力和反應時(shí)間作為重點(diǎn)考察的因素,進(jìn)行系列的單因素試驗和正交試驗,確定了4-(6-甲氧基-2-萘基)-1,3-丁二酮催化加氫制備萘丁美酮的優(yōu)化反應條件。以四氫呋喃為溶劑,催化劑Pd/C(10%)用量10%,對甲苯磺酸用量2%,氫氣壓力0.4 MPa,40℃下反應4 h,產(chǎn)品收率達88.3%,純度99.1%。 |
關(guān)鍵詞:萘丁美酮;催化加氫;正交試驗 |
中圖分類(lèi)號:R977.1 文獻標識碼:A 文章編號:1009-9212(2007)05- 0037-03 |
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Preparation of Nabumetone by Catalytic Hydrogenation |
LI Wei-wei1,2,TONG Guo-tong1,L?譈 Lu-ping1
(1. Chemical Department,Hangzhou Vocational and Technical College,Hangzhou 310018,China;2. College of Chemical Engineering and Material Science,Zhejiang University of Technology,Hangzhou 310014,China) |
Abstract:Nabumetone was prepared from 4-(6-methoxy-2-naphthyl)-1,3- butandione by catalytic hydrogenation. Main interacting factors such as catalyst,solvent,dehydrating agent,temperature,pressure and reaction time were studied. The optimum conditions were as follows:40℃,0.4 MPa,Pd/C(10%)as catalyst,THF as solvent,2% p-toluene sulfonic acid as dehydrating agent and reaction time 4 hours. Under above conditions,the yield of nabumetone was up to 88.3% with the purity of 99.1% after recrystallization. |
Key words:nabumetone;catalytic hydrogenation;orthogonal design |
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作者簡(jiǎn)介:李巍。1980-),男,湖北孝感人,助教,碩士研究生,研究方向:精細有機中間體合成。(E-mail:zgdlwwwwl@163.com)
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收稿日期:2007-06-05
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