Restudy of "dimethylstibinoborine"
Restudy of "dimethylstibinoborine"
复制标题
“二甲基锑硼烷”的再研究
DOI：
10.1021/ic50167a051
复制
发表时间：
1977
影响因子：
4.6
通讯作者：
A. Burg
中科院分区：
文献类型：
--
作者：
A. Burg
217反应被观察到形成一个白色的NH4CI云和黄色的，有时是棕色的聚合物。3气体反应产物的红外光谱显示，在1362和1261 cm™1处的强红外波段监测表明，总有相当数量的SO2与hnso一起形成。在透光灵敏度模式5t（透光尺度扩大5倍）下，可见光谱在500 ~ 400 nm区域呈现振动结构。这种结构表明存在少量的噻嗪酰氯，即在红外光谱中无法检测到的NSC1。在第二种方法中，涉及“较低”的压力，首先将NH3加入到1-1中。反应球在约30托的压力下。然后通过真空线将亚硫酰氯蒸气缓慢地加入到反应球中，以达到所需的约10 Torr的化学计量量。使用该方法，未形成棕色聚合物，仅观察到少量黄色聚合物。红外光谱分析表明，SO2的含量非常少，所得的HNSO产率与“高”压法所得的HNSO产率相当。即使将仪器的灵敏度模式从5倍增加到10倍，可见光谱也没有由于NSC1而出现任何吸收带。
Correspondence Inorganic Chemistry, Vol. 16, No. 1, 1977 217 reaction was observed by the formation of a white cloud of NH4CI and of yellowishand sometimes brownish polymers. 3 The infrared spectrum of the gaseous reaction product always showed the formation of considerable amounts of SO2 together withHNSO as evidenced by monitoring the intense infrared bands at 1362 and 1261 cm™ 1, respectively. The visible spectrum exhibited vibronic structure in the region 500-400 nm on transmittance sensitivity mode 5 T (tran-smittance scale expanded 5 times). This structure10 was indicative of the presence of small amounts of thiazyl chloride, NSC1, which was not detectable in the infrared spectrum. In the second method, involving “lower” pressures, NH3 was first added to the 1-1. reaction bulb at a pressure of about 30 Torr. Thionyl chloride vapor was then added slowly to the reaction bulb through the vacuum line to achieve the required stoichiometric amount of about 10 Torr. By use of thismethod, no brown polymer was formed and only a small amount of the yellow polymer was observed. The infrared spectrum showed that a very small amount of SO2 was present and that the yield of HNSO was comparable to the yield of HNSO produced by the “higher” pressure method. The visible spectrum did not exhibit any absorption bands due to NSC1 even by doubling the sensitivity mode of the instrument from 5 to 10.