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磷酰胺和磷酰胺硫醚的合成与表征及其与钯(II)配合物的配位。

Synthesis and Characterization of Phosphinecarboxamide and Phosphinecarbothioamide, and Their Complexation with Palladium(II) Complex.

机构信息

Department of Chemistry, Graduate School of Science, Osaka Metropolitan University, Sumiyoshi-ku, Osaka 558-8585, Japan.

Department of Chemistry, Graduate School of Science, Osaka City University, Sumiyoshi-ku, Osaka 558-8585, Japan.

出版信息

Molecules. 2022 Aug 29;27(17):5564. doi: 10.3390/molecules27175564.

DOI:10.3390/molecules27175564
PMID:36080329
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9457633/
Abstract

Reactions of isocyanates/isothiocyanates with primary and secondary phosphines without solvent at room temperature afforded phosphinecarboxamide/phosphinecarbothioamide, respectively, in excellent yields. Furthermore, palladium complex Pd(COD)Cl was allowed to react with PhPC(O)NHPh () to afford [Pd{PhPC(O)NHPh-κ}Cl] (). On the other hand, the reaction of Pd(COD)Cl with 1 eq. of PhPC(S)NHPh () afforded [PdCl{PhPC(S)NHPh-κ}] (). In the case of a 1:2 molar ratio, [PdCl{PhPC(S)NHPh-κ}{PhPC(S)NHPh-κ}]Cl () was formed. The newly obtained compounds were fully characterized using multielement NMR measurements and elemental analyses. In addition, the molecular structures of PhPC(O)NH(CH)Cl (), PhPC(S)NHPh(4-Cl) (), and - were determined using single-crystal X-ray diffraction.

摘要

异氰酸酯/异硫氰酸酯与伯膦和仲膦在室温下无需溶剂反应，分别以优异的收率得到了相应的膦酰胺/膦硫酰胺。此外，钯配合物 Pd(COD)Cl 与 PhPC(O)NHPh（）反应，得到了[Pd{PhPC(O)NHPh-κ}Cl]（）。另一方面，Pd(COD)Cl 与 1 eq. 的 PhPC(S)NHPh（）反应，得到了[PdCl{PhPC(S)NHPh-κ}]（）。当摩尔比为 1:2 时，形成了[PdCl{PhPC(S)NHPh-κ}{PhPC(S)NHPh-κ}]Cl（）。新得到的化合物通过多元素 NMR 测量和元素分析进行了充分的表征。此外，PhPC(O)NH(CH)Cl（）、PhPC(S)NHPh(4-Cl)（）和-的分子结构通过单晶 X 射线衍射确定。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/7663b28eb54e/molecules-27-05564-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/c4f27ba4339e/molecules-27-05564-g001.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/e6547b78e828/molecules-27-05564-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/efc54d93aee7/molecules-27-05564-sch005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/6a26b0f81a89/molecules-27-05564-sch006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/174999b9a159/molecules-27-05564-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/7db278f60787/molecules-27-05564-sch007.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/7663b28eb54e/molecules-27-05564-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/c4f27ba4339e/molecules-27-05564-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/f6cd41d55429/molecules-27-05564-sch001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/236371d7200e/molecules-27-05564-sch002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/aff2aca5a7df/molecules-27-05564-sch003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/904eba78a3ae/molecules-27-05564-sch004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/e6547b78e828/molecules-27-05564-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/efc54d93aee7/molecules-27-05564-sch005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/6a26b0f81a89/molecules-27-05564-sch006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/174999b9a159/molecules-27-05564-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/7db278f60787/molecules-27-05564-sch007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/986f29877cef/molecules-27-05564-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/784ce8d30472/molecules-27-05564-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/085b/9457633/7663b28eb54e/molecules-27-05564-g006.jpg

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