Cameron Jones, P. Junk, M. L. Cole
2001
Citations
1
Influential Citations
8
Citations
Journal
Main Group Metal Chemistry
Abstract
Experimental Preparation of [AlH2Cl(Quinuclidine)2]: Solid quinuclidine hydrochloride (1.55g, 10.5 mmol) was added to a stirred slurry of L1AIH4 (0.2g, 5.3 mmol) in diethyl ether (40 cm) sustained at a temperature of -50°C. The resultant colourless slurry was then warmed to room temperature over 5hrs, by which time gas evolution had ceased. Volatiles were removed in vacuo to yield an oily white solid that was subsequently recrystallised from diethyl ether. Placement at -30°C overnight gave the title compound as colourless prisms. Yield 1.19g, 79%; mp 182°C (dec). ' H NMR (400 MHz, C 6 D 6 , 300K): δ 1.12 (12H, m, CH2), 1.24 (2H, m, CH), 2.64 (12H, t, JHH 9.2 Hz, NCH2), 4.22 (2H, br s, Al-Η). | 3 C NMR (100.6 MHz, C 6 D 6 , 300K): δ 19.8 (s, CH), 27.6 (s, CH2) , 56.3 (s, NCH2). MS EI: m/z (%) 176 [{M-Quin}+, 100], 251 [{M-C1}+, 64], 111 [Quin+, 42], IR (Nujol)v/ cm . 1691 cm" (s,br, Al-H).