995-32-4Relevant articles and documents
4-(diethoxy-phosphoryl)-2-methyl-but-2-enoate preparation method
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Paragraph 0076; 0077, (2020/01/25)
The invention discloses a 4-(diethoxy-phosphoryl)-2-methyl-but-2-enoate preparation method, which comprises: (a) carrying out an oxidation reaction on a pyruvic aldehyde aqueous solution to obtain a pyruvic acid/pyruvate aqueous solution; and (b) carrying out a reaction on the pyruvic acid/pyruvate aqueous solution and tetraethyl ethylene diphosphate, and performing an esterification reaction withan alcohol to obtain 4-(diethoxy-phosphoryl)-2-methyl-but-2-enoate. The method of the invention has advantages of cheap and easily available raw materials, simple operation of each step, high yield of the whole route, and high industrial application value.
A Universally Applicable Methodology for the Gram-Scale Synthesis of Primary, Secondary, and Tertiary Phosphines
Rinehart, N. Ian,Kendall, Alexander J.,Tyler, David R.
supporting information, p. 182 - 190 (2018/02/06)
Although organophosphine syntheses have been known for the better part of a century, the synthesis of phosphines still represents an arduous task for even veteran synthetic chemists. Phosphines as a class of compounds vary greatly in their air sensitivity, and the misconception that it is trivial or even easy for a novice chemist to attempt a seemingly straightforward synthesis can have disastrous results. To simplify the task, we have previously developed a methodology that uses benchtop intermediates to access a wide variety of phosphine oxides (an immediate precursor to phosphines). This synthetic approach saves the air-free handling until the last step (reduction to and isolation of the phosphine). Presented herein is a complete general procedure for the facile reduction of phosphonates, phosphinates, and phosphine oxides to primary, secondary, and tertiary phosphines using aluminum hydride reducing agents. The electrophilic reducing agents (iBu)2AlH and AlH3 were determined to be vastly superior to LiAlH4 for reduction selectivity and reactivity. Notably, it was determined that AlH3 is capable of reducing the exceptionally resistant tricyclohexylphosphine oxide, even though LiAlH4 and (iBu)2AlH were not. Using this new procedure, gram-scale reactions to synthesize a representative range of primary, secondary, and tertiary phosphines (including volatile phosphines) were achieved reproducibly with excellent yields and unmatched purity without the need for a purification step.
Flexible diphosphonic acids for the isolation of uranyl hybrids with heterometallic UVI = O - ZnII cation-cation interactions
Tian, Tao,Yang, Weiting,Wang, Hao,Dang, Song,Sun, Zhong-Ming
supporting information, p. 8288 - 8290 (2013/09/02)
A family of uranyl diphosphonates have been hydrothermally synthesized using various flexible diphosphonic acids and Zn(UO2)(OAc) 4·7H2O in the presence of bipy or phen. Single-crystal X-ray analyses indicate that these compounds represent the first examples of uranyl phosphonates with heterometallic UVI = O - Zn II cation-cation interactions.
