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With water; dihydrogen peroxide In dichloromethane at 0℃; for 4 h;
Compound 8 (5.0 g, 9.3 mmol) was melted in 100 mL of CH2C12, and H2O2 (30 percent, 4.0 mL, 186 mmol) was dropped therein while the mixture was being ice bathed. This mixture was stirred for 4 hours. The reactant was quenched with distilled water after stirring, and CH2C12 extraction was performed 3 times. An organic layer was dried with anhydrous magnesium sulfate, and the solvent was distilled off. An obtained solid was purified by a reprecipitation method with use of hexane, which yielded a compound 9 (white powder, 5.0 g, 94 percent). IR (ATR) 1183 (st, P=O), 1070-1226 (st, C-O-C) cm-11H NMR (300 MHz, CDCl3, 25 °C) 87.06-7.71 (m, 26H, Ar), 6.02-6.07 (m, 2H, Ar) ppm 31P NMR (200 MHz, CDCl3, 25 °C) 826.41 (2P) ppm FAB-Mass(m/z) = 571 [M+H]+.
84%
With dihydrogen peroxide In tetrahydrofuran at 20℃; for 2 h;
General procedure: Synthesis of the phosphine oxidesThe phosphine oxides were synthesized by oxidation ofthe corresponding phosphines. Calculated amounts of H2O2(30percent) were added slowly to the vigorously stirred THF solutionof the respective phosphine. Stirring was maintainedat room temperature for 2 h. After evaporation of THF, theresidue was treated with acetone-ethyl acetate to obtain therespective phosphine oxide product as a precipitate. The precipitatesthus obtained were filtered off and dried in a vacuum.All melting points were above 360 C with decomposition. DPEPO: 1H NMR (250 MHz, CDCl3): d = 7:75 – 7:64(m, 9H, Phen-H), 7.42 (m, 13H, Phen-H), 7.05 – 7.04 (t, 2H,Phen-H), 7.07 (t, 2H, Phen-H), 7.08 (t, 2H, Phen-H). – MS(EI): m=z = 570. Yield 84percent.
Reference：
[1] Chemistry - A European Journal, 2011, vol. 17, # 2, p. 521 - 528
[2] Patent: EP2471799, 2012, A1, . Location in patent: Page/Page column 16
[3] Zeitschrift fur Naturforschung - Section B Journal of Chemical Sciences, 2014, vol. 69, # 2, p. 239 - 247
[4] Chemistry - A European Journal, 2013, vol. 19, # 1, p. 141 - 154
[5] Patent: JP2018/35101, 2018, A, . Location in patent: Paragraph 0086; 0087
2
[ 101-84-8 ]
[ 808142-23-6 ]
Reference：
[1] Chemistry - A European Journal, 2013, vol. 19, # 1, p. 141 - 154
3
[ 1079-66-9 ]
[ 808142-23-6 ]
Reference：
[1] Chemistry - A European Journal, 2013, vol. 19, # 1, p. 141 - 154
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