ChemicalBook CAS DataBase List TRIS(TRIMETHYLSILYL)PHOSPHITE

TRIS(TRIMETHYLSILYL)PHOSPHITE synthesis

11synthesis methods

Product Name:TRIS(TRIMETHYLSILYL)PHOSPHITE
CAS Number:1795-31-9
Molecular formula:C9H27O3PSi3
Molecular Weight:298.54

By silylation of anhydrous phosphorous acid (dried by repeated azeotropic evaporation of a solution in THF with dry benzene) with excess Chlorotrimethylsilane and excess Triethylamine in dimethoxyethane, toluene, or Et2O-THF, followed by evaporation of the solvent and vacuum distillation of the residue. The residue, which contains a mixture of tris(trimethylsilyl) phosphite and bis(trimethylsilyl) phosphonate [HP(O)(OTMS)2], can also be heated with sodium (140 °C, 13-22 h), followed by vacuum distillation to obtain pure tris(trimethylsilyl) phosphite.

14468-90-7 Synthesis

14468-90-7
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$49.20/10g

1795-31-9
150 suppliers
$17.50/0.5g

Yield:1795-31-9 0.13 mol

Reaction Conditions:

with phosphorous acid in tetrahydrofuran at 70; for 4 h;

Steps:

2
Weigh 0.05mol phosphorous acid,Adding 0.15mol of 3-trimethylsilylpyrrolidone,THF is dissolved,Reaction was performed at 70 ° C for 4h.Filtered to give pyrrolidone as a solid,Wash three times with 30ml of petroleum ether,Combined petroleum ether phases,Remove the solvent,GC-MS test.9g was distilled under reduced pressure,Colorless transparent liquid.After adding sodium metal,The reaction was protected under nitrogen at 140 -150 for 20h under anhydrous conditions.After cooling, distilled under reduced pressure,Tris (trimethylsilyl) phosphite was obtained in an amount of 0.13 mol (20 mmHg, 75 ° C).

References:

Weihong Force System (Huzhou) Co., Ltd.;He Wei;Dong Jian;Fei Zhenyu;Zhang Zhigang;Wen Juan·liu·maidisi CN110551151, 2019, A Location in patent:Paragraph 0078; 0079

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999-97-3 Synthesis