第 37 卷第 5 期Vol. 37 No. 5
2007 年 10 月Oct 2007

所属栏目:医药及中间体

催化加氢制备萘丁美酮工艺研究
李巍巍1,2,童国通1,吕路平1 (1.杭州职业技术学院 化工系,浙江 杭州 310018;2.浙江工业大学 化学工程与材料学院,浙江 杭州 310014)
摘 要:选取催化剂、溶剂、脱水剂、温度、压力和反应时间作为重点考察的因素,进行系列的单因素试验和正交试验,确定了4-(6-甲氧基-2-萘基)-1,3-丁二酮催化加氢制备萘丁美酮的优化反应条件。以四氢呋喃为溶剂,催化剂Pd/C(10%)用量10%,对甲苯磺酸用量2%,氢气压力0.4 MPa,40℃下反应4 h,产品收率达88.3%,纯度99.1%。
关键词:萘丁美酮;催化加氢;正交试验
中图分类号:R977.1  文献标识码:A  文章编号:1009-9212(2007)05- 0037-03
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
作者简介:李巍巍(1980-),男,湖北孝感人,助教,硕士研究生,研究方向:精细有机中间体合成。(E-mail:zgdlwwwwl@163.com)
收稿日期:2007-06-05