35696-40-3Relevant academic research and scientific papers
Preparation method of m-aminophenylacetylene
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Paragraph 0008; 0021, (2021/05/29)
The invention discloses a preparation method of m-aminophenylacetylene, belonging to the technical field of organic synthesis. The method comprises the following steps of: subjecting m-nitroacetophenone serving as a raw material to reacting with triethyl phosphite under the action of a catalyst, continuously converting the m-nitroacetophenone into enol form, and condensing the enol form with the triethyl phosphite to obtain condensation ester, wherein the condensation ester is easy to separate and high in purity, m-nitrophenylacetylene is generated from the ester under the action of strong base, and m-aminophenylacetylene is generated from the ester through reduction. Compared with an acetophenone chlorination method, the method of the invention has the advantages that phosphorus oxychloride does not need to be used for changing oxygen of the m-nitroacetophenone into chlorine, pollution is small, purity is high ( 98% or more), the use of high-pollution raw material reagents is avoided, operation is simple, the environment-friendly effects are realized, and industrial production can be conveniently realized.
An efficient separation method for enol phosphate and corresponding β-ketophosphonate from their mixtures under aqueous conditions
Moorhoff, Cornelis M.
, p. 2069 - 2086 (2007/10/03)
Separation of a mixture β-ketophosphonate 3 and their corresponding enol phosphate 4 is efficiently carried out in aqueous alkaline solutions. Enol phosphate 4 is first extracted with hexanes:dichloromethane (19:1). Acidification of the aqueous layer followed by extraction of the β-ketophosphonate 3 with dichloromethane completes the separation. Thus, when 1-bromo-2,4-pentadione la reacted with triethyl phosphite to give diethyl (2,4-dioxopentyl)phosphonate 3a (Arbuzov-product) and the corresponding enol phosphate 4a (Perkow-product), separation of the two compounds was carried out using this method.
