Transition Metals in Organic Synthesis*
Transition Metals in Organic Synthesis*
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DOI：
10.1055/s-1976-24126
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发表时间：
1976-12
期刊：
影响因子：
--
通讯作者：
A. Kozikowski;H. Wetter
中科院分区：
文献类型：
--
作者：
A. Kozikowski;H. Wetter
在氩气下，在室温搅拌下，向四羰基四氢呋喃二钠（11 mmol）的四氢呋喃（50 ml）溶液中加入酸四氢呋喃（11 mmol）的四氢呋喃（10 ml）溶液。20分钟后，将反应混合物用冰醋酸（1.2ml）处理，减压蒸馏除去反应溶剂，残余物用0.5N氢氧化钠水溶液（50 ml）萃取并过滤。将滤液酸化并用三份乙醚（70 ml）萃取，将有机层干燥（Na 2SO 4）并浓缩。残余物通过重结晶纯化或转化为2，4-二硝基苯腙。邻苯二甲酸酐（19）得到邻苯二甲酸（20），产率为61%.
To disodium tetracarbonyl lerratc (ll mmol) in tetrahydroluran (50 ml) was added the acid arlhydridc (ll mmol) in tctrzihydrofuran (10 ml] with stirring at room temperature under argon. After 20 min, the reaction mixture was treated with glacial acetic acid (1.2 ml), the reaction solvent was removed by distillation at reduced pressure, and the residue was extracted with 0.5 N aqueous sodium hydroxide (50 ml) and filtered. The filtrate was acidified and extracted with three portions of ether (70 ml), and the organic~ layer dried (Na2SO4) and concentrated. The residue was purified by recrystallization or was converted into a 2, 4-dinitrophenylhy drazone. Phthalic anhydride (19) gave phthalaldehydic acid (20) in 61 ‘I-{Y yield.