* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With 1% Au/TiO2; water In ethyl acetate at 25℃; for 0.5h;
With Perbenzoic acid In benzene at 45℃;
With Perbenzoic acid In benzene at 45℃;
With dimethyl sulfoxide In 1,4-dioxane at 5℃; Irradiation;
With Perbenzoic acid In benzene at 45℃;
5 %Spectr.
With chloro[meso-tetrakis(p-trifluoromethylphenyl)porphyrinato]cobalt(III) In chloroform at 25℃; for 200h;
Reactions of Disilane
General procedure: Typically, a mixture of 5.0 ×10-3 mmol of disilane,6 5 ×10-4 mmolof CoIIICl-Por, and 5.0 ×10-3 mmol of dodecane as an internal standard in 0.5 mL of chloroformwas allowed to stand at 25°C. The reaction progress was monitored by GC and the productwas analyzed by GC-MS. To observe the intermediates, a mixture of 1.0 ×10-2 mmol ofdisilane, 5 ×10-4 mmol of CoIIICl-Por in 0.5 mL of deuteriochloroform was placed in an NMRtube. Anaerobic reaction was carried out in the sealed NMR tube using deuteriochloroformdried over activated molecular sieves 4A and degassed by freeze-pump-thaw as the solvent.
With carbon dioxide; cesium fluoride In N,N-dimethyl-formamide at 110℃; for 1.5h; Schlenk technique;
cis-bis(dimethylphenylsilyl)bis(methyldiphenylphosphine)platinum[ No CAS ]
[ 768-32-1 ]
[ 778-24-5 ]
[ 1145-98-8 ]
Yield
Reaction Conditions
Operation in experiment
1: 82.9%
2: 0%
3: 0%
With P(C6H5)2CH3 In benzene-d6 heating in benzene-d6 soln. in a sealed NMR tube (80°C, 40 h) with addn. of diphenylmethylphosphine (8 equiv. per Pt-complex); further products: polymers; detn. by GLC;
1: 81.3%
2: 0%
3: 0%
With P(C6H5)2CH3 In benzene-d6 heating in benzene-d6 soln. in a sealed NMR tube (80°C, 40 h) with addn. of diphenylmethylphosphine (2 equiv. per Pt-complex); further products: polymers; detn. by GLC;
1: 65.6%
2: 12.6%
3: 5.2%
With P(C6H5)2CH3 In benzene-d6 heating in benzene-d6 soln. in a sealed NMR tube (80°C, 40 h) with addn. of diphenylmethylphosphine (0.5 equiv. per Pt-complex); further products: polymers; detn. by GLC;
1: 50.3%
2: 27.2%
3: 12%
With P(C5H6)2CH3 In benzene-d6 heating in benzene-d6 soln. in a sealed NMR tube (80°C, 40 h); further products: polymers; detn. by GLC;
1: 48.7%
2: 28.6%
3: 19.1%
In benzene-d6 heating in benzene-d6 soln. in a sealed NMR tube (80°C, 40 h); further products: polymers; detn. by 1H-NMR;
With tetrabutyl ammonium fluoride; water In dimethyl sulfoxide at 80℃; for 24h; Schlenk technique;
II. Typical Procedure for Formic Acid Synthesis form CO2, H2O, and Disilane
To a glass reactor equipped with a CO2 balloon was added tetrabutylammonium fluoride trihydrate (TBAF*3H2O, 5.0×10-2 mmol), tetramethyldiphenyldisilane (0.50 mmol), water (3.1 mmol), and DMSO (1 mL). The resulting reaction mixture was stirred vigorously at 80 °C. The products were confirmed by the comparison of their GC-MS spectra and 1H NMR spectra with those of authentic data. The yields were determined by the internal standard technique using a CDCl3 solution of the reaction mixture. Figure S1 shows the 1H NMR spectrum of a CDCl3 solution of the reaction mixture after 24 h. Mesitylene or triisopropylbenzene was used as the internal standard.
Stage #1: 1,2-diphenyltetramethyldisilane With potassium <i>tert</i>-butylate; hydrogen In tetrahydrofuran-d8 for 1h;
Stage #2: With hydrogen; C62H51N2Ni2(1-)*K(1+)*2C4H10O2 In tetrahydrofuran-d8 at 60℃; for 18h;
Stage #1: racemic methyl phenyl sulfoxide; (dimethyl(phenyl)silyl)zinc chloride With bis(triethylphosphine)nickel(II) bromide In tetrahydrofuran at 80℃; for 0.0833333h; Schlenk technique; Inert atmosphere;
Stage #2: In tetrahydrofuran at 80℃; for 0.5h; Schlenk technique; Inert atmosphere;