10.1002/adsc.202000817
Advanced Synthesis & Catalysis
desired product was isolated by flash chromatography (97:3
n-pentane:diethyl ether).
Musaev, M. S. Sigman, H. M. L. Davies, ACS Catal.
2018, 8, 678-682.
Kinetic isotopic effect: Following the general methodology
described for small scale catalysis, to a solution of the
[Fe(Fpda)(THF)]2 (2.5 mol%) in dichloromethane (1 mL)
was added ethyl diazoacetate (0.16 mmol) followed by the
addition of a 1:1 mixture of cyclohexane and cyclohexane-
d12 (0.04 mmol each). LiAl(ORF)4 [ORF= (OC(CF3)3]
(0.08mmol) was then introduced and the reaction was stirred
at 40 °C for 1 hour. After that time, the resulting solution
was filtered through a silica plug to remove paramagnetic
impurities and the sample was analyzed by GC and GC-MS.
16% of product yield was determined by GC. The ratio of
P1 and P1-d12 gave a KIE value of 1.94.
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Axial/equatorial
functionalization
determination:
Axial/equatorial isomers of reaction crudes containing P5-
C3, P5-C4, P7-C3 and P7-C4 were determined by
comparison of their NMR data with those registered of
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Acknowledgements
We acknowledge STR of UdG for experimental support. This work
was supported by the Spanish Ministry of Science, Innovation and
Universities (PGC2018-101737-B-I00 to M.C. and Generalitat de
Catalunya (2017 SGR 00264 and ICREA Academia Award to
M.C.) and Comunidad de Madrid Research Talent Attraction
Program (2018-T1/AMB-11478 to A. H.-G.).
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