865-47-4Relevant articles and documents
Unusual Reactivity of Silicon Grease Towards Metal Alkoxides: Serendipity for Structural Chemistry
Nahrstedt, Vanessa,Raauf, Aida,Hegemann, Corinna,Brune, Veronika,Schl?fer, Johannes,Mathur, Sanjay
, p. 1102 - 1109 (2021)
Controlled synthesis of moisture sensitive metal alkoxides demands the use of silicon grease for the inert synthetic manipulation of starting materials using glass apparatus to avoid adventitious hydrolysis. Spontaneous reaction of the siloxane units (?OSi(Me3)2)n) with the synthesized alkoxides often leads to molecular metal alkoxides based siloxane frameworks. These spontaneous incorporation of siloxane units into homo- and heterometallic alkoxide building blocks lead to the new multinuclear homo- and heterometallic alkoxide-siloxide compounds [Ce2(OtBu)4{Me2Si(OtBu)O}2(NO3)2] (1), [Zr{(OiPr)2{Me2SiO2}Sr{Zr2(OiPr)8}}2] (2) and [Sn2In2O2{Me2Si(OiPr)O}(OiPr)5]2 (3). Multifunctional coordination properties of these siloxane units enable the molecular approach to synthetically demanding polymetallic complexes for potential MOx-SiOx nanocomposites fabrication.
Efficient Synthesis of N-Substituted 2,4-Azepandione Ring System as an Active Intermediate for Heterocyclic Syntheses
Waly, Mohamed A.,Yossif, Shiam A.,Ibrahim, Ismail T.,Sofan, Mamdouh A.
, p. 1318 - 1326 (2017/03/27)
An improved efficient synthesis for 2,4-azepandiones (3, 8, and 14) could be achieved by a careful control of the reaction conditions to cyclize ethyl 4-(N-acetylarylamino) butanoate (1, 7, and 13), respectively. The ethyl 4-arylamino butanoate (9 or 12) was prepared by stirring the ethyl 4-bromobutanoate and substituted anilines at room temperature. Then, they were acetylated with acetyl chloride and triethylamine under the conditions that avoid the formation of 2-pyrrolidinone derivatives 10. Due to the rapid decomposition of the acetylated product (7 or 13) to its starting material (9 or 12), the reaction mixture is directly transferred without workup to the next cyclization step. The azepandione synthesis is favored by using a weak base at low temperature, where it is in a competition with the other modes of ring closure. The structures of the new compounds were supported by correct analytical and spectral data.
Preparation method for low residual granular sodium alkoxide or potassium alcoholate
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Paragraph 0039-0040, (2017/01/17)
The invention provides a preparation method for low residual granular sodium alkoxide or potassium alcoholate. The method includes using sodium or potassium and alcohol as raw materials, mixing the mixture with a solvent, reacting in inert gas atmosphere by using a microwave heating method, and removing the residual alcohol and solvent in the presence of microwave after the reaction to get the granular sodium alkoxide or potassium alcoholate. The microwave frequency is 2450 +/- 50 MHz. The method can prepare sodium alkoxide or potassium alcoholate with low residual solvent, and the prepared sodium alkoxide or potassium alcoholate is large granular solid, so that the development from powdered product to granular product can be realized, and the problems of residual solvent and potential risk troubled human for a long time can be overcome.
