806. []20 (nm): -488?(589) (c 0.235, CHCl3). (S p )-2-[(R)-1-Diphenylphosphinoethyl]-(S p )-2-diphenylphosphino-1,1-biferrocene ((R,Sp,Sp)-2). To a degassed answer of crude (R,Sp,Sp)-9 (500 mg, 0.626 mmol) in THF (5 mL) had been added PMHS (0.430 mL) and Ti(O-iPr)four (711.9 mg, two.50 mmol). The resulting mixture was heated beneath reflux beneath argon at 75 for four h. The resulting dark green answer was cooled to area temperature and transferred to the top of a column (aluminum oxide, PE/EA/EtOH = 85/15/1) with out prior workup. Elution and subsequent removal in the solvents gave the crude item as an orange strong. As a way to eliminate excess PMHS, the crude product was suspended in PE/EA (95/5) and filtered. The product was washed quite a few occasions together with the exact same solvent mixture and was dried in vacuo (yield: 340 mg, 4.38 mmol, 70 ). Mp: 89 . 1H NMR (600 MHz, CD2Cl2): 1.50 (dd, J1 = 7.1 Hz, J2 = 12.2 Hz, 3H, CH3CH), 3.26-3.33 (m, 1H, CH3CH), 3.85 (s, 5H, Cp), four.13-4.15 (m, 1H, H3/H5), 4.14 (s, 5H, Cp), 4.19-4.21 (m, 3H, H3 + H5 + H4), four.48 (dt, J1 = 0.six Hz, J2 = 2.6 Hz, 1H, H4), four.57-4.59 (m, 1H, H3/H5), 7.02-7.07 (m, 2H, PhB-ortho), 7.10-7.16 (m, 2H, PhD-ortho), 7.17-7.21 (m, 2H, PhB-meta), 7.22-7.28 (m, 3H, PhD-meta + PhB/D-para), 7.33-7.38 (m, 4H, PhA-meta + PhApara + PhB/D-para), 7.38-7.41 (m, 3H, PhC-meta + PhC-para), 7.47- 7.52 (m, 2H, PhA-ortho), 7.65-7.70 (m, 2H, PhC-ortho). 13C1H NMR (150.9 MHz, CD2Cl2): 20.2 (d, J = 9.9 Hz, CH3CH), 28.6 (dd, J1 = three.two Hz, J2 = 7.eight Hz, CH3CH), 66.eight (C4), 67.7 (d, J = ten.9 Hz, C3/C5), 69.9 (C4), 70.0 (d, J = 11.five Hz, C3/C5), 70.45 (5C, Cp/Cp), 70.47 (5C, Cp/Cp), 72.7 (d, J = four.3 Hz, C3/C5), 73.five (d, J = 15.four Hz, C1), 75.1 (bs, C3/C5), 83.6 (bs, C1), 91.1 (d, J = 29.0 Hz, C2), 91.9 (C2), 128.2-128.8 (10C, 8Ph-meta + 2Ph-para), 129.four (Ph-para), 129.8 (bs, Ph-para), 132.9 (d, J = 14.1 Hz, 2C, PhB-ortho), 133.0 (d, J = 17.5 Hz, 2C, PhA-ortho), 135.2 (d, J = 19.five Hz, 2C, PhD-ortho), 135.78 (d, J = 23.1 Hz, 2C, PhC-ortho), 139.7 (d, J = 11.7 Hz, PhC-ipso), 141.5 (d, J = ten.9 Hz, PhA-ipso), PhB-ipso and PhD-ipso not observed. 31P1H NMR (243 MHz, CD2Cl2): -24.five (Fc-PPh2), 7.1 (CH3CH-PPh2). HR-MS (ESI, MeOH/MeCN): m/z [M]+ calcd 766.1304 for C46H40Fe2P2, found 766.1308. []20 (nm): -481?(589) (c 0.245, CHCl3). (S p )-2-[(R)-1-Diphenylphosphinoethyl]-(S p )-2-diphenylphosphino-1,1-biferrocene-P,P-bis(borane) ((R,S p ,S p )-2?2BH3).2089292-48-6 Chemscene The derivative (R,Sp,Sp)-2 (100 mg, 0.Buy152835-00-2 126 mmol) was dissolved in THF (two mL), as well as the solution was degassed. Towards the resulting solution was added dropwise at 0 a resolution of BH3 in THF (1 M, 0.38 mL, 0.38 mmol), and also the mixture was stirred for 16 h at space temperature The reaction mixture was quenched at 0 with water (15 mL) and extracted twice with DCM.PMID:23074147 The combined organic phases have been washed with water, dried more than MgSO4, and filtered, as well as the solvents have been evaporated. The desired solution was obtained as an orange foam (yield: one hundred.9 mg, 0.125 mmol, 99 ). Single crystals suitable for X-ray structure determination have been grown from CH2Cl2/ ethyl acetate by slow evaporation with the solvent. Mp: 180 dec. 1H NMR (400 MHz, CDCl3): 0.86-1.90 (6H, BH3), two.19 (dd, J1 = 7.2 Hz, J2 = 17.4 Hz, 3H, CH3CH), three.77 (s, 5H, Cp), 3.80 (t, J = two.6 Hz, H4), three.86-3.89 (m, 1H, H3), three.96 (s, 5H, Cp), four.00-4.04 (m, 1H, H3), 4.05-4.16 (m, 1H, CH3CH), 4.36-4.42 (m, 1H, H3), four.44 (t, J = two.six Hz, H4), four.64-4.68 (m, 1H, H5), 7.34-7.87 (m, 20H, Ph). 13 C1H NMR (one hundred.6 MHz, CDCl3): 23.7 (d, J = five.4 Hz, CH3CH),.