Compound 1
1-(2,6-diisopropylphenyl)-3,3,5,5-tetramethylpyrrolidine-2-ylidene beryllium dichloride
From: Neutral zero-valent s-block complexes with strong multiple bonding
View in PubChem | 1H NMR | 9Be NMR | 13C NMR | Cyclic Voltammogram | CIF | MDL Molfile | ChemDraw
Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.
Synthesis of [Be(MeL)Cl2], 1: A suspension of BeCl2 (212 mg, 2.6 mmol, 1.1 eq.) in benzene (20 mL) was treated with MeL (638 mg, 2.2 mmol, 1.0 eq.) and stirred at room temperature for 5 h. The reaction mixture was filtered and the filtrate dried in vacuo. The resulting solid was washed with hexane (3 x 10 mL) and recrystallized from benzene at 4 °C, affording 1 as a colorless crystalline solid (642 mg, 79%). 9Be NMR (C6D6, 56 MHz): δ = 12.9 (s). 1H NMR (C6D6, 500 MHz): δ = 7.08 (t, JHH = 8 Hz, 1H, CHpara), 6.98 (d, JHH = 8 Hz, 2H, CHpara), 2.69 (sept., JHH = 7 Hz, 2H, C H (CH3)2), 1.49 (d, JHH = 7 Hz, 6H, CH(C H3)2), 1.45 (s, 6H, CH3), 1.33 (s, 2H, CH2), 1.07 (d, JHH = 7 Hz, 6H, CH(C H3)2), 0.82 (s, 6H, CH3). 13C{1H} NMR (C6D6, 125 MHz): δ = 145.5 (Cq), 133.1 (Cq), 130.4 (CHpara), 128.3 (Cq), 125.6 (CHmeta), 82.3 (Cq), 54.5 (Cq), 50.3 (CH2), 29.2 (C H(CH3)2), 28.61 (CH3), 28.59 (CH3), 27.2 (CH( C H3)2), 24.7 (CH( C H3)2). Elemental analysis calcd (%) for C20H31BeCl2N: C 65.74, H 8.55, N 3.83; found: C 66.20, H 8.63, N 3.91. Crystal data for 1: C20H31BeCl2N, Mr = 365.37, colorless block, 0.26×0.19×0.15 mm3, monoclinic space group P21/n, a = 22.883(13) Å, b = 9.955(3) Å, c = 28.329(9) Å, β = 105.871(18)°, V = 6208(5) Å3, Z = 12, ρcalcd = 1.173 g ・ cm–3, μ = 0.315 mm–1, F(000) = 2352, T = 100(2) K, R1 = 0.0672, wR2 = 0.0974, 12694 independent reflections [2θ≤52.744°] and 673 parameters.
