Organic metals. Novel route to cycloalkenotetrathiafulvalenes
Organic metals. Novel route to cycloalkenotetrathiafulvalenes
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有机金属。
DOI：
10.1021/jo00866a041
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发表时间：
1976
影响因子：
3.6
通讯作者：
A. Garito
中科院分区：
文献类型：
--
作者：
H. Spencer;M. Cava;F. G. Yamagishi;A. Garito
1.2. 3-将硒二唑（150 mg）加入100 ml 0.01 N叔丁醇钾的叔丁醇溶液中。气体逸出停止后，将所得的I溶液通过毛细管缓慢加入500 ml醇中，历时8-9小时，其中已加入足够的乙酸以使溶液在整个反应过程中保持微酸性。加入所有I后，在旋转薄膜蒸发器上在40 ℃浴温下将醇蒸发至接近干燥。将分离的固体（一些富烯和盐）离心，并将上清液在50 g硅胶上用10%氯仿的石油醚溶液（bp 40-60）进行色谱分析。硒酮以黄色条带移动，正好在相应的富烯后面洗脱。产率取决于I的加入速度。根据其在紫外线下的吸光度判断，在非常稀的溶液中可以获得几乎定量的产率。然而，分离的纯酯的产率约为50%。致谢。这项工作得到了伊朗科学和高等教育部的部分支持。
1.2. 3-Selenadiazole (150 mg) was added to a 100-ml solutionof 0.01 N potassium tert-butoxide in tert-butyl alcohol. After the gas evolution ceased, the resulting solution of I was added slowly through a capillary tube, over 8-9 hr, to 500 ml of alcohol, to which enough acetic acid had been added to keep the solutionslightly acidic throughout the reaction. After all of I had been added the alcohol was evaporated to near dryness on a rotary film evaporator at 40 bath temperature. The solid that separated (some fulvene and salts) was centrifuged and the supernatant liquid was chroma-tographed on 50 g of silica gel, using 10% chloroform in petroleum ether (bp 40-60). The selenonesters moved as yellow bands, being eluted just behind the corresponding fulvenes. The yields depended on the speed of addition of I. Nearly quantitative yields could be obtained in very dilute solution, as judged by their absorbance in the uv. Yields of isolated pure esters, however, were about 50%.Acknowledgment. This work was supported, in part, by the Ministery of Science and Higher Education of Iran.