摘要
研究了标题化合物的合成新工艺。以双环戊二烯为起始原料,首先与25%的硫酸(n(双环戊二烯)∶n(硫酸)=1∶1)进行水合反应制得3a,4,5,6,7,7a-六氢-5-羟基-4,7-桥亚甲基茚,收率达82%;其次用5%Pd/C作为催化剂对3a,4,5,6,7,7a-六氢-5-羟基-4,7-桥亚甲基茚进行加氢反应制得2,3,3a,4,5,6,7-7a-八氢-5羟基-4,7-桥亚甲基茚,收率90%;最后用30%过氧化氢(n(2,3,3a,4,5,6,7-7a-八氢-5羟基-4,7-桥亚甲基茚)∶n(过氧化氢)=1∶2)氧化加氢产物得到标题化合物,收率84%,反应总收率在58%以上。该过程条件温和,操作简单,污染小,具有工业化应用前景。
Cyclopentanonorcamphor was synthesized from di- cyclopentadiene via three steps. The first step is hydration re- action,followed by hydration with 25% sulfuric acid to form intermediate 1 with 82% yield. The molar ratio of dicyclopen- tadiene to sulfuric acid is 1： 1. The second step is hydrogena- tion of the intermediate 1 using 5% Pd/C as the catalyst,and the intermediate 2 was obtained with 90% yield. The third step is oxidation the hydrogenated product with 30% H202 to provide the target compound with 84% yield. The molar ratio of intermediate 2. The total yield is over 58% and the advan- tages of the present procedure are easy operation, mild reac- tion condition and low pollution. Thus, it can be expected to have a good prospect for industrial application.
出处
《化学试剂》
CAS
CSCD
北大核心
2012年第11期1047-1049,共3页
Chemical Reagents
