Compound 2
2-(2,6-diisopropylphenyl)-3,3-dimethyl-2-azaspiro[4,5]decan-1-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(CyL)Cl2], 2: A suspension of CyLHBF4 (400 mg, 1.0 mmol, 1.0 eq.) in benzene (3 mL) was treated with a solution of NaN(SiMe3)2 (177 mg, 1.0 mmol, 1.0 eq.) in benzene (5 mL). The reaction was stirred at room temperature for 30 min before the mixture was filtered. The filtrate was treated with BeCl2 (2 x 77 mg, 2.0 mmol, 2.0 eq.) and stirred at room temperature for 1 h. After filtration the solution was reduced in vacuo and stored at 4 °C, affording 2 as a colorless crystalline solid (167 mg, 43%). 9Be NMR (CD2Cl2, 56 MHz): δ = 12.8 (s). 1H NMR (CD2Cl2, 500 MHz): δ = 7.45 (t, JHH = 8 Hz, 1H, CHpara), 7.30 (d, JHH = 8 Hz, 2H, CHmeta), 2.77 (sept., JHH = 7 Hz, 2H, C H (CH3)2), 2.42–2.37 (m, 2H, CH2,cy), 2.15 (s, 2H, CH2), 1.84–1.74 (m, 2H, CH2,cy), 1.65 (m, 2H, CH2,cy), 1.47–1.36 (m, 3H, CH2,cy),1.41 (s, 6H, CH3), 1.32 (d, JHH = 7 Hz, 6H, CH(C H3)2), 1.31 (d, JHH = 7 Hz, 6H, CH(C H3)2).13C{1H} NMR (CD2Cl2, 125 MHz): δ = 238.9 (Cq,carbene), 145.7 (Cq), 133.4 (Cq),130.4 (CHpara), 125.8 (CHmeta), 83.1 (Cq), 60.6 (Cq), 45.6 (CH2), 35.5 (CH2,cy), 30.0 (CH3),29.2 (C H(CH3)2), 27.0 (CH( C H3)2), 25.3 (CH2,cy), 25.0 (CH( C H3)2), 22.2 (CH2,cy). Elemental analysis calcd (%) for C23H35BeCl2N: C 68.13, H 8.70, N 3.45; found: C 68.48, H 8.87,N 3.20. Crystal data for 2: C23H35BeCl2N, Mr = 405.43, colorless plate, 0.23×0.16×0.06 mm3, orthorhombic space group Pbca, a = 20.214(6), b = 9.634(4), c = 23.524(6) Å, V = 4581(3) Å3, Z = 8, ρcalcd = 1.176 g cm–3, μ = 0.291 mm–1, F(000) = 1744, T = 100(2) K, R1 = 0.0342, wR2 = 0.0885, 3994 independent reflections (1.73≤2θ≤ 26.37o) and 250 parameters.
