Table 3. Measured product distribution (in %) of fluorosilicates obtained by 19F-NMR signal integration after >36 h in CD2Cl2 between the reactants given in column 1 a .
[F-Si(catX)2]– + Si(catY)2 | [F-Si(catX)2]– | [F-Si(catY)2]– | [F-Si(catX) (catY)]– | rel. FIAsol |
X = H, Y = tBu | 65 | <1 | 35 | H > tBu |
X = tBu, Y = H | <1 | 70 | 30 | |
X = H, Y = F | 20 | 76 | 4 | F > H |
X = F, Y = H | >99 | <1 | 0 | |
X = tBu, Y = F | <1 | 72 | 28 | F > tBu |
X = F, Y = tBu | >99 | <1 | <1 | |
X = F, Y = Cl | 21 | 27 | 52 | Cl > F |
X = Cl, Y = F | 49 | 8 | 43 | |
X = F, Y = Br | 17 | 30 | 53 | Br > F |
X = Br, Y = F | 55 | 5 | 40 | |
X = Cl, Y = Br | 20 | 29 | 51 | Br > Cl |
X = Br, Y = Cl | 58 | 4 | 38 |
a0.05 M of [K@18-c-6][F-Si(catX)2] and 0.05 M Si(catY)2 in CD2Cl2, room temp., min. 36 h equilibration time, for Y = Cl and Br, the CH3CN adducts were used.