L1(5 mol%),1a(0.3 mmol),2a(0.1 mmol), Ph3P (2.0 equiv.), KHCO3 (0.4 equiv.), acetone/MeCN (2 mL, v/v = 1:1, 0.05 M), blue LEDs, ambient temperature, 12 h. [b] Yields were determined by gas chromatography (GC) analysis using dodecane as an internal standard. DMF = N, N...
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随后,作者以苯并磷戊环2a和对甲基碘苯3a作为模板底物来探索钯催化的C-H芳基化过程(Table 1)。通过一系列条件筛选,作者发现当反应使用Pd(OAc)2(5 mol%),NaOtBu (2.0 equiv),甲苯做溶剂,微波条件下90 ℃下反应1小时,可以以79%的产率实现C-H芳基化产物4aa的合成(Table 1, entry 14)。此外,当此反应放大至...
p -Tolyl–I (1.1 equiv.), Pd(PPh3)2Cl2 (5 mol%), Na2CO3 (2.0 equiv.), THF/H2O, 60 °C,12h. Isolated yield: 90% iii. MeOTf (1.1 equiv.), CH2Cl2, r.t. 2h. Isolated yield: 95% Me b iv. PhSnMe3 (2a), standard coupling conditions. 1m iv 1m 2a 3ma (92%) Me O Me ...
When 20 equiv 4-bromoacetophenone were added to a thawing solution of 2 (Fig. 4b), the resulting EPR spectrum could be simulated with two sets of parameters corresponding to two different species in a 0.6:1 ratio and that were tentatively assigned to the initial NiI species and a new Ni...
The reaction of Fc#BBr2 with 2 equiv of Et3SiH gives the boron-bridged dinuclear species Fc#2BBr with concomitant liberation of B2H6 (Fc# = (C5Me5)Fe(C5H4)). The transformation is slow (48 h) but nevertheless provides yields of >85%. Fc#2BBr can conveniently be converted into t...
Treatment of (t-)BuN=TiCl(2)Py(3) with 2 equiv lithium ketiminate compound, Li[OCMeCHCMeN(Ar)] (where Ar = 2,6-diisopropylphenyl), in toluene at room tempe... SH Hsu,JC Chang,CL Lai,... - 《Inorganic Chemistry》 被引量: 41发表: 2004年 ...
However, when TEMPO (3.0 equiv.) was added to the standard reaction, the desired cycloaddition product E1 could be obtained with a maintained yield (95%), and G1 was detected with only 1% yield. The negligible influence of TEMPO on this reaction may be attributed to the quick ISC of 1,...
Treatment of the Ni(II) and Cu(II) complexes with 3 equiv of trityl tetrafluoroborate in acetonitrile results in oxidative dehydrogenation, yielding the 15-π cations [M(MeHMe-2,9-diene)]+ (15) which were isolated as their ... TJ Truex,RH Holm - 《Journal of the American Chemical Soci...
The treatment of Cp3Ln with 1 equiv of N,N′-dicyclohexyl-N′′-phenylguanidine followed by reacting with butyllithium yields a series of novel guanidinate dianion complexes of heterobimetallic lanthanide−lithium with formula Cp2Ln[(CyN)2CNPh]Li(THF)3 (Ln = Yb (1a), Er (1b), Y (...