GOVDI et al.
7 of 8
|
795 (vs), 860 (w), 919 (w), 953 (w), 976 (w), 1018 (m), 1057
(w), 1138 (s), 1207 (s), 1254 (s), 1327 (s), 1377 (s), 1454
(m), 1497 (s), 1585 (w), 1620 (w), 1643 (w), 1708 (w), 1829
(w), 1890 (w), 1948 (w), 3005 (s), 3047 (s). Anal. Calcd. for
C30H21P: C, 87.36; H, 5.13%. Found: C, 87.19; H, 5.08%.
ACKNOWLEDGMENTS
Synthesis of the starting phosphine ligand was carried out
according to State contract (Grant No. 01201061738) using
the equipment of the Baykal Analytical Centre for Collective
Use, SB RAS. A.I.G. and S.F.V. thank RFBR for financial
support (Grant No. 16-03000589a).
4.2
General procedure for cross-
|
coupling of alkynes 2 with iodoarenes 1
ORCID
4.2.1 Method A and B
|
A mixture of alkyne 2 (0.5 mmol), 1-iodoarene 1 (0.5 mmol),
CuI (4.75 mg, 0.025 mmol), K2CO3 (103.5 mg, 0.75 mmol),
and Ph3P or Np3P (0.05 mmol) in DMF (4 mL) was stirred
under an argon atmosphere at 120°C. The reaction mixture
was cooled and diluted with EtOAc and washed with solution
of NH4Cl, and dried over Na2SO4. The solvents were evapo-
rated under reduced pressure. After working-up the reaction
mixture samples were analyzed by GC-MS.
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4.2.2
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|
Np3PO0.24·DMSO
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γ = 120°, V = 4057.5(11) Å3, Z = 6, dcalc = 1.21 g/cm3,
μ = 0.202 mm−1, (2θ)max = 54.94°, a total number of reflec-
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