background and overview[1]
1,5-cycloctadiene bis(methylbiphenylphosphine)iridium hexafluorophosphate abbreviation [ir(cod)(pmeph2)2] pf6, is an iridium metal catalyst. there are reports in the literature that it can further react with 2,2-bipyridine to form another iridium metal catalyst [ir(bipy)h2(prph2) 2] pf6.
apply[1-2]
[ir(cod)(pmeph2)2] pf6 preparation of [ir(bipy)h2 sub>(prph2)2] the method of pf6 is as follows:
combine [ir(cod)(pmeph2)2] pf6 (1 equivalent, 286.3 mg, 0.338 mmol) and 2 ,2-bipyridine (1 equiv, 53.0 mg, 0.338 mmol) was dissolved in degassed ch2cl2 (10 ml). the resulting red solution was cooled to 0°c. dihydrogen gas was bubbled in with constant stirring for 20 minutes. diethyl ether (100 ml) was added dropwise to the orange solution to precipitate 250.9 mg of beige solid (82.9%), which was obtained by vacuum filtration and dried under vacuum. recrystallize with ch2cl2/et2o.
1h nmr (cd2cl2, 298 k): δ h (ppm) 8.46 (dd, 3j2,3 = 5.4, ??5j2,5 = 0.7, 2), 7.93 (d, 3j5,4 = 8.0, 5), 7.87 (ddd, 3j4,3 = 7.5, 3j4,5 = 8.2, 4j4,2 = 1.5, 4), 7.33 (m, p), 7.25 (m, o and m), 7.08 (ddd, 3j3,4 = 7.1, 3j3,2) 5.5, 4j3,5 = 1.4, 3), 1.88 (t harris,17b |2jh,p + 4jh,p| = 6.4, pmeph2), -19.87 (t, 2jh,p = 16.8, h). 13c{1h} nmr (cd2cl2, 298 k): δ c (ppm) 155.9 (s, 6), 155.4 (s, 2), 137.5 (s, 4), 133.4 (t, 1jipso,p = 26.7, ipso), 132.0 (t, 2jo,p = 6.0, o), 130.5 (s, p), 128.7 (t, 3jm,p = 5.0, m), 127.5 (s, 3), 123.8 (s, 5), 17.0 (t, |1jc,p + 3jc, p| = 37.6, pmeph2). 31p{1h} nmr (cd2cl2, 298 k): δ p (ppm) -0.27 (s, pmeph2), -143.14 (sept, 1jp,f = 711.0, pf6 -). 19f nmr (cd2cl2, 298 k): δ f (ppm) -73.50 (d,1jf,p = 711.0, pf6 -). ir (thin film, cm-1 ): ν(ir-h) 2176.1, ν(pf6) 836.2. anal. calcd for c36h36irn2p3f6: c, 44.62; h, 3.84; n, 2.74. found: c, 44.58; h, 4.14; n, 2.75. yield: 82.9%.
report 2,
albinati a et al. reported that [ir(cod)(pmeph2)2] pf6 can be further prepared [(eta5- c5h5)m(mu-h)2(mu-(eta5:eta1-c5h4))irh(pmeph2)2][bph4] (m = mo and w).
