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CAS No. : | 104413-90-3 | MDL No. : | N/A |
Formula : | C34H28Cl2FeP2Pt | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | PUPHKEOCQOWYKL-UHFFFAOYSA-L |
M.W : | 820.36 | Pubchem ID : | 145707322 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P264-P280-P302+P352-P337+P313-P305+P351+P338-P362+P364-P332+P313 | UN#: | N/A |
Hazard Statements: | H315-H319 | Packing Group: | N/A |
GHS Pictogram: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
56% | With N(C2H5)3 In dichloromethane stirred for 24 h at room temp. under Ar atm.; evapd.; column chromy.; recrystd. (CHCl3/methanol); elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium hydroxide; In ethanol; chloroform; at 20℃; for 3h; | 2.3 [PdCl(sac)(kappa2-dppf)] (2) A warm ethanol (10 cm3) solution of sodium saccharinate (0.112 g, 0.55 mmol) was added to a chloroform (20 cm3) solution of [PdCl2(kappa2-dppf)] (0.20 g, 0.27 mmol). Following a similar procedure to above, [PdCl(sac)(kappa2-dppf)] (2) was isolated as a red-brown crystalline solid in 83% yield. 1H NMR: delta 8.31-7.01 (m, 24H, Ar), 4.32 (br, 4H, CH), 3.42 (br, 4H, CH); 31P{1H} NMR: delta 37.20 (d, JPP 12.7 Hz), 28.99 (d, JPP 12.7 Hz). IR nu/cm-1; IR(KBr) 3058w, 3051w, 2972w, 2918w, 1670s, 1586m, 1433m, 1294s, 1247s, 1155vs, 962m, 482s cm-1; Elemental Anal. Calc. for PdFeSNClP2O3C41H32: C, 56.06; H, 3.67; N, 1.59. Found: C, 56.26; H, 3.40; N, 1.70%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
72% | In ethanol; chloroform at 20℃; for 3h; | 2 General 2.2 [PtCl(sac)(κ2-dppf)] (1) A warm ethanol (10 cm3) solution of sodium saccharinate (0.096 g, 0.47 mmol) was added to a chloroform (20 cm3) solution of [PtCl2(κ2-dppf)] (0.20 g, 0.23 mmol). The turbid yellow mixture was stirred at room temperature for 3 h then filtered. The filtrate was set aside to evaporate slowly at room temperature. The yellow crystals of [PtCl(sac)(κ2-dppf)] (1) thus formed were filtered off and dried under vacuum (0.17 g, 72% yield). 1H NMR: δ 8.13-6.93 (m, 24H, Ar), 5.35 (s, 1H, CH), 4.89 (s, 1H, CH), 4.67 (s, 1H, CH), 4.54 (s, 1H, CH), 4.45 (s, 1H, CH), 4.38 (s, 1H, CH), 4.19 (s, 1H, CH), 3.44 (s, 1H, CH), 3.38 (s, 1H, CH); 31P{1H} NMR: δ 15.30 (JPP 14.5, JPtP 3820 Hz), 6.01 (JPP 14.5, JPtP 3605 Hz). IR ν/cm-1; IR(KBr) 3058w, 3016w, 2925w, 2860w, 1766s, 1587m, 1434m, 1299s, 1249s, 1161vs, 960m, 480s cm-1; Elemental Anal. Calc. for PtFeSNClP2O3C41H32: C, 50.92; H, 3.34; N, 1.45. Found: C, 51.00; H, 3.50; N, 1.60%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Stage #1: [1,1'-bis(diphenylphosphino)ferrocene]platinum(II) chloride; silver trifluoromethanesulfonate In dichloromethane for 3h; Schlenk technique; Glovebox; Darkness; Stage #2: diphenyl-(6-methyl-pyridin-2-yl)phosphine In dichloromethane Schlenk technique; Glovebox; Overall yield = 90 %; Overall yield = 354 mg; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | In dichloromethane; at 20℃; for 3h; | PtCl2(dppf) (100.0mg, 0.122mmol) was dissolved in deaerated CH2Cl2 (12.0mL). Thereafter was added successively P(OPh)3 (31.9muL, 0.122mmol) and Na(BArF4) (108.0mg, 0.122mmol) at room temperature. The obtained suspension was stirred for 3h at room temperature, followed by its filtration and concentration of the clear red solution to dryness. Yield: 202.9mg (85%). Elemental analysis calculated for C84H55BClF24O3P3PtFe (1957.9): C, 51.53%; H, 2.81%: Found: C, 51.45%; H, 3.03%. 1H NMR (400MHz, 294K, CDCl3, ppm): 3.5 (m, 3JPH=2Hz, 4JPH=2Hz, 2H, Cp-H), 4.3 (br. s, 2H, Cp-H), 4.5 (m, 3JPH=2Hz, 4JPH=2Hz, 2H, Cp-H), 4.5 (br. s, 2H, Cp-H), 6.9-7.6 (m, 35H, Ar-H), 7.6+7.8 (s, 12H, ArF-H). 13C{1H} NMR (100MHz, 294K, CDCl3, ppm): 74.6 (d, 3JPC=7Hz, Cp-C), 75,1 (d, 3JPC=9Hz, Cp-C), 75.8 (d, 2JPC=10Hz, Cp-C), 76.4 (d, 2JPC=12Hz), ipso-C(Cp), hidden by CHCl3,117.6-161.6 (m, Ph-C), 124.5 (q, 1JCF=273Hz, CF3). 31P{1H} NMR (162MHz, 294K, CDCl3, ppm): 14.9 (dd, 2JPP=13Hz, 2JPP=29Hz, 1JPtP=3583Hz, dppf), 22.2 (dd, 2JPP=13Hz, 2JPP=651Hz, 1JPtP=2542Hz, dppf), 73.9 (dd, 2JPP=29Hz, 2JPP=651Hz, 1JPtP=4249Hz, P(OPh)3). |