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Synthesis And Characterization Of 5-butyl-5-ethyl-2-chloro-1, 3, 2-dioxaphosphorinane

Posted on:2008-08-10Degree:MasterType:Thesis
Country:ChinaCandidate:N JuFull Text:PDF
GTID:2121360245493367Subject:Chemical processes
Abstract/Summary:PDF Full Text Request
1,3,2-dioxaphosphorinane compounds show the unique dioxane–phosphorus–heterocyclic structrue which formed as active unit of these compounds, they have become hot points in organophosphate chemicals applied research field. 1,3,2-dioxaphosphorinane which is an important intermediates in fine chemical industry, can be widely used in pesticides, flame retardants, antioxidant and biological materials, and other fields.The properties of 5 -ethyl- 5-butyl- 2- chloro-1,3,2-dioxaphosphorinane were introduced , the applications of 1,3,2-dioxaphosphorinane were summarized. The route of synthesis BEOP from phosphorus trichloride and BEPD in the present of CH2Cl2 was determined , the factors which effect on the reaction and yield such as material ratio, reaction time and temperature, dropping time and solvent percentage were inspected; the optimal reaction conditions : n (BEPD) : n (PCl3) 1:1, the reaction temperature 10°C, dropping time 30 minutes, reaction time 2 hours, solvent percentage 60% were ascertained. The suitability and stability of the obtained technological conditions have confirmed through L9(34) orthogonal experiment and repetition. The products of BEPD reacted with PCl3 were analyzed by gas chromatography, mass spectrometry and nuclear magnetic resonance spectroscopy, the structure of one by-product was determined. Under these conditions, BEOP yield over 96%. The structure of BEOP was identified by infrared spectroscopy, mass spectrometry and nuclear magnetic resonance spectroscopy for the first time.The possible mechanism of the reaction was also discussed, which was classified as SN2 nucleophilic substitution reactions.
Keywords/Search Tags:1,3-propanediol, 1,3,2-dioxaphosphorinane, synthesis, characterization, S_N2 nucleophilic substitution
PDF Full Text Request
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