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16
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33745911774
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note
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1H NMR spectrum of the crude product revealed a 3:1 mixture of 4 and 5. The residue was subjected to column chromatography [Merck Silica gel 60 (0.063-0.100)] using n-hexane-ethyl acetate 9:1, followed by n-hexane-ethyl acetate 4:1 as eluent. In the initial fractions, 4 was obtained (122 mg, after trituration with n-hexane, as a pale-yellow crystalline powder, mp 114-115 °C, yield 59%); this was followed by mixed fractions, and then by 5 (29 mg, after trituration with n-hexane, as a white crystalline powder, mp 127-133 °C, yield 14%).
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17
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0003053061
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Lempert K., Nyitrai J., Zauer K., Kálmán A., Argay Gy., Duisenberg A.J.M., and Sohár P. Tetrahedron 29 (1973) 3565-3569
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Nyitrai, J.2
Zauer, K.3
Kálmán, A.4
Argay, Gy.5
Duisenberg, A.J.M.6
Sohár, P.7
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18
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37049072029
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Foces-Foces C., Llamas-Saiz A.L., Claramunt R.M., López C., and Elguero J. J. Chem. Soc. Chem. Commun. (1994) 1143-1145
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Elguero, J.5
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0001571865
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Böcskei Zs., Simon K., Rao R., Caron A., Rodger C.A., and Bauer M. Acta Cryst. C54 (1998) 808-810
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Böcskei, Zs.1
Simon, K.2
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22
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0000130956
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Bauer M., Harris R.K., Rao R.C., Apperley D.C., and Rodger C.A. J. Chem. Soc., Perkin Trans. 2 (1998) 475-481
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24
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33745892261
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note
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15N HMBC spectra; their accuracy was approximately ±1 ppm. All spectra were measured by using the standard pulse programs installed by Bruker.
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25
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33745920649
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note
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3): -51.4 (N-1).
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26
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33745899185
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note
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3): -258.5 (N-1).
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27
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33745907123
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note
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Electron ionization mass spectra experimental. The 70 eV low-resolution spectra were recorded on a VG ZABSpec instrument equipped with an OPUS V3.3 data system. The samples were introduced through a solid-inlet system without heating the probe. The accelerating voltage was 8 kV, the temperature of the source was 433 K, and the trap current was 200 μA. The accurate mass measurements were performed by voltage scanning at a resolution of 6000-10,000, using perfluorokerosene as reference compound.
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28
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33745904032
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note
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+: 77(6).
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29
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33745907695
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note
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+: 77(7).
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