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小小丸子

银虫 (小有名气)

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专业: 环境微生物学

[交流] 求助～～～亚磷酸三甲酯

请问亚磷酸三甲酯（制有机磷类农药的中间体）的合成，实验室怎样做合成实验？
反应物是：甲醇，三氯化磷，三乙胺
溶剂是：苯

请高人相告，本人实验遇到困难，想寻求好的合成实验操作方案。谢谢！

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xiaoxiaodu

木虫 (小有名气)

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Trimethyl phosphite, 9CI, 8CI
Synonym(s): Trimethoxyphosphine. Trimethoxyphosphorus(III). Trimethoxophosphorus(III)
Chapman  Hall Number: JRL60-C
CAS Registry Number: 121-45-9
Type of Compound Code(s): AC1040
P(OMe)3

Molecular Formula: C3H9O3P
Molecular Weight: 124.076
Accurate Mass: 124.028932
Percentage Composition: C 29.04%; H 7.31%; O 38.68%; P 24.96%
Use/Importance: Reagent for dehydrohalogenations, debrominations and deoxygenations, used in Corey-Winter synth. Uses similar to those of Triethyl phosphite JQR76-I
Physical Description: Air-sensitive liq. with powerful sickly odour
Melting Point: Mp 78
Boiling Point: Bp 111-112. Bp23 22
Density: d204 1.05
Refractive Index: n20D  1.4080
Other Data: Forms complexes with cuprous halides
Hazard  Toxicity: Flammable. Powerful obnoxious odour. Induces headache. Severe skin and eye irritant. Corrosive and irritating to tissues of the respiratory tract. LD50 (rat, orl) 1600 mg/kg. OES: long-term 2 ppm
RTECS Accession Number: TH1400000

Aldrich: 32632-1
Fluka: 92723
Sigma:
References:
Aldrich Library of FT-IR Spectra, 1st edn., 1985, 1, 910A, (ir)
Aldrich Library of 13C and 1H FT NMR Spectra, 1992, 1, 1465C, (nmr)
Aldrich Library of FT-IR Spectra: Vapor Phase, 1989, 3, 838B, (ir)
Meyrick, C.I. et al., J.C.S., 1950, 225, (ir, Raman)
Halman, M. et al., J.C.S., 1963, 2853, (uv)
Goodell, L.J. et al., Can. J. Chem., 1969, 47, 2461, (pmr)
Verstuyft, A.N. et al., Inorg. Chem., 1976, 15, 732-734, (cmr, pmr)
Cowley, A.H. et al., Inorg. Chem., 1977, 16, 854-860; 1984, 23, 3378, (pe)
Griend, L.J.V. et al., J.A.C.S., 1977, 99, 2459, (props, struct)
Gray, G.A. et al., J.A.C.S., 1977, 99, 3243, (nmr)
Labintsev, V.B. et al., Zh. Org. Khim., 1977, 13, 1141-1144; J. Org. Chem. USSR (Engl. Transl.), 1977, 13, 1050, (ms)
Organophosphorus Reagents in Org. Synth., (J.I.G. Cadogan, Ed.), Academic Press, 1979, (uses)
Chattopadhyay, S. et al., J. Electron Spectrosc. Relat. Phenom., 1981, 24, 27-36, (pe)
Vasil'ev, V.V. et al., Zh. Obshch. Khim., 1981, 51, 2134-2135; J. Gen. Chem. USSR (Engl. Transl.), 1981, 51, 1836, (O-17 nmr)
Worley, S.D. et al., J. Electron Spectrosc. Relat. Phenom., 1982, 25, 135-147, (struct)
Sodhi, R.N. et al., J. Electron Spectrosc. Relat. Phenom., 1983, 32, 283-312, (struct, pe)
Krudoper, S.A. et al., J. Fluorine Chem., 1983, 22, 305-344, (pe)
Cload, P.A. et al., Org. Mass Spectrom., 1983, 18, 57-59, (ms)
Bart, J.C.J. et al., Phosphorus Sulfur Relat. Elem., 1983, 17, 205-220, (conformn, complexes)
Holtzclaw, J.R. et al., Org. Mass Spectrom., 1985, 20, 90, (ms, struct)
Nefedev, V.I. et al., J. Electron Spectrosc. Relat. Phenom., 1988, 46, 381-404, (Auger, pe)
Wils, E.R.J. et al., Fresenius' Z. Anal. Chem., 1990, 338, 22-27, (ms)
Dahn, H. et al., Magn. Reson. Chem., 1992, 30, 1089-1096, (O-17 nmr)
Gu, M. et al., Org. Mass Spectrom., 1993, 28, 1135-1143, (ms)
Encyclopaedia of Reagents for Organic Synthesis, (ed. Paquette, L.A.), Wiley, 1995, 7, 5217-5220, (use)
Bretherick, L., Handbook of Reactive Chemical Hazards, 4th edn., Butterworths, 1990, 1238
Luxon, S.G., Hazards in the Chemical Laboratory, 5th edn., Royal Society of Chemistry, 1992, 1291
Lewis, R.J., Sax's Dangerous Properties of Industrial Materials, 8th edn., Van Nostrand Reinhold, 1992, TMD500

[00091508-1] A20 C0 N0 M0 R84