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Self-assembly of Keggin-type U(VI)-containing tungstophosphates with a sandwich structure: an efficient catalyst for the synthesis of sulfonyl pyrazoles
Inorganic Chemistry Frontiers ( IF 6.1 ) Pub Date : 2021-08-26 , DOI: 10.1039/d1qi00485a Guo-Ping Yang 1 , Xing-Lei Zhang 1 , Yu-Feng Liu 1 , Dong-Di Zhang 2 , Ke Li 1 , Chang-Wen Hu 3
Inorganic Chemistry Frontiers ( IF 6.1 ) Pub Date : 2021-08-26 , DOI: 10.1039/d1qi00485a Guo-Ping Yang 1 , Xing-Lei Zhang 1 , Yu-Feng Liu 1 , Dong-Di Zhang 2 , Ke Li 1 , Chang-Wen Hu 3
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The reaction of UO2(OAc)2 and Na9[A-PW9O34] in solution with different pH values leads to the formation of two Keggin-type sandwich polyoxometalates, namely Na11H(H2O)31[Na(UO2)(A-PW9O34)]2·7H2O (1) and Na12(H2O)29[Na(UO2)(A-PW9O34)]2·7H2O (2), which have been characterized by single-crystal X-ray diffraction, FT-IR spectroscopy, and PXRD techniques. Compounds 1 and 2 crystallize in similar conditions with different pH values and show similar sandwich crystal structures except that one extra Na(I) ion acts as a bridging linker in compound 2 than in 1. It is notable that 1 exhibits excellent catalytic activity for the synthesis of sulfonyl pyrazoles via the condensation and cyclization reaction of sulfonyl hydrazides with 1,3-diketones, and the yield of the desired product is up to 99%. This is the first report to investigate the catalytic properties of U-containing polyoxometalates.
中文翻译：
具有夹心结构的Keggin型U（VI）磷钨磷酸盐的自组装：合成磺酰基吡唑的有效催化剂
UO 2 (OAc) 2和Na 9 [A-PW 9 O 34 ]在不同pH值的溶液中反应，形成两种Keggin型夹心多金属氧酸盐，即Na 11 H(H 2 O) 31 [Na (UO 2 )(A-PW 9 O 34 )] 2 ·7H 2 O ( 1 ) 和 Na 12 (H 2 O) 29 [Na(UO 2 )(A-PW 9 O 34 )] 2 ·7H 2 O ( 2)，已通过单晶 X 射线衍射、FT-IR 光谱和 PXRD 技术表征。化合物1和2在具有不同 pH 值的类似条件下结晶，并显示出类似的夹心晶体结构，除了一个额外的 Na( I ) 离子在化合物2 中充当桥连键，而不是在1 中。值得注意的是，1通过磺酰肼与1,3-二酮的缩合和环化反应合成磺酰吡唑表现出优异的催化活性，目标产物的产率高达99%。这是第一份研究含 U 多金属氧酸盐催化性能的报告。
更新日期：2021-09-08
中文翻译：
具有夹心结构的Keggin型U（VI）磷钨磷酸盐的自组装：合成磺酰基吡唑的有效催化剂
UO 2 (OAc) 2和Na 9 [A-PW 9 O 34 ]在不同pH值的溶液中反应，形成两种Keggin型夹心多金属氧酸盐，即Na 11 H(H 2 O) 31 [Na (UO 2 )(A-PW 9 O 34 )] 2 ·7H 2 O ( 1 ) 和 Na 12 (H 2 O) 29 [Na(UO 2 )(A-PW 9 O 34 )] 2 ·7H 2 O ( 2)，已通过单晶 X 射线衍射、FT-IR 光谱和 PXRD 技术表征。化合物1和2在具有不同 pH 值的类似条件下结晶，并显示出类似的夹心晶体结构，除了一个额外的 Na( I ) 离子在化合物2 中充当桥连键，而不是在1 中。值得注意的是，1通过磺酰肼与1,3-二酮的缩合和环化反应合成磺酰吡唑表现出优异的催化活性，目标产物的产率高达99%。这是第一份研究含 U 多金属氧酸盐催化性能的报告。
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