1023-63-8Relevant academic research and scientific papers
Mono and double Mizoroki-Heck reaction of aryl halides with dialkyl vinylphosphonates using a reusable palladium catalyst under aqueous medium
Lee, Han-Sheng,Pai, Shao-Hsuan,Liao, Wei-Ting,Yang, Xin-Jing,Tsai, Fu-Yu
, p. 34293 - 34299 (2017)
Operationally-simple and reusable Pd-catalyzed mono and double Mizoroki-Heck reactions of aryl halides and dialkyl vinylphosphonates using iPr2NH as a base in aqueous medium under air were developed. For aryl iodides, the reaction could be conducted at 80 °C under a low catalyst loading (0.1-1 mol%). When aryl bromides were applied, however, a greater amount of catalyst (5 mol%) and a longer reaction time at 120 °C were required. Simply changing dialkyl vinylphosphonates as the limiting reagent led to the formation of 2,2-diaryl vinylphosphonates in good to high yields. After reaction, the residual aqueous solution could be reused for both mono and double Mizoroki-Heck reactions, making the reactions greener and reducing wastage of precious metals and use of harmful organic solvents as the reaction medium.
Synthesis and Characterization of Pd exchanged MMT Clay for Mizoroki-Heck Reaction
Srivastava, Vivek
, p. 605 - 613 (2018/07/31)
We successfully synthesized Pd@MMT clay using a cation exchange process. We characterized all the synthesized Pd@MMT clays using sophisticated analytical techniques before testing them as a heterogeneous catalyst for the Mizoroki - Heck reaction (mono and double). The highest yield of the Mizoroki-Heck reaction product was recovered using thermally stable and highly reactive Pd@ MMT-1 clay catalyst in the functionalized ionic liquid reaction medium. We successfully isolated 2-aryl-vinyl phosphonates (mono-Mizoroki-Heck reaction product) and 2,2-diaryl-vinylphosphonates (double-Mizoroki-Heck reaction product) using aryl halides and dialkyl vinyl phosphonates in higher yields. The low catalyst loading, easy recovery of reaction product and 8 times catalyst recycling are the major highlights of this proposed protocol.
Preparation method of olefin phosphate compound
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Paragraph 0018; 0019; 0030; 0031, (2017/08/28)
The invention discloses a preparation method of an olefin phosphate compound. The method comprises the following steps: arylethylene and phosphate according to a mol ratio 1:4-6 are used as raw materials; ferric chloride and copper salt are used as catalysts, and di-tert-butyl peroxide is used as an oxidizing agent; the raw materials and triethylamine are mixed, an organic solvent is added, and under the protection of inert gas, a reaction is carried out at 90-110 DEG C; after the reaction ends, washing is carried out, rotary evaporation is used for removing the solvent, and column chromatography is carried out in order to obtain the olefin phosphate compound. Base metal copper and iron are used as catalysts, reactant arylethylene and phosphate have low price, toxicity is low, the oxidizing agent is green and environmentally friendly, and the yield of the synthetic reaction of the olefin phosphate compound is high.
