118
T. Kusukawa, W. Ando / Journal of Organometallic Chemistry 561 (1998) 109–120
2C), 143.50 (s, 2C), 143.99 (s, 2C), 144.16 (s, 2C),
145.32 (s, 2C), 145.38 (s, 2C), 145.99 (s, 2C), 146.05 (s,
2C), 146.10(s, 2C), 146.15 (s, 2C), 146.40 (s, 2C), 146.63
(s, 2C), 146.97 (s, 2C), 147.42 (s, 2C), 147.72 (s, 2C),
148.58 (s, 2C), 150.38 (s, 2C), 152.82 (s, 2C), 162.92 (s,
2C), 165.37 (s, 2C); 29Si-NMR (60 MHz, 1:1 CDCl3–
CS2) l 5.55; FAB MS 1186–1189 (M+ +1 cluster);
UV–vis (toluene) umax (nm): 533 (br).
144.62 (s, 1C), 144.87 (s, 1C), 145.26 (s, 1C), 145.31 (s,
1C), 145.37 (s, 1C), 145.50 (s, 1C), 145.65 (s, 1C),
146.09 (s, 1C), 146.36 (s, 1C), 146.41 (s, 1C), 146.49 (s,
1C), 146.64 (s, 1C), 146.74 (s, 1C), 146.84 (s, 1C),
147.58 (s, 1C), 147.74(s, 1C), 148.28 (s, 2C), 148.60(s,
1C), 152.88 (s, 1C), 153.26 (s, 1C), 154.24 (s, 1C),
156.83 (s, 1C); 29Si-NMR (80 MHz, 1:1 CDCl3–CS2) l
6.17; MALDI-TOF-MS: 1907 (M+).
1
4f: brown solid; 1H-NMR(500 MHz, 1:1 CDCl3–
CS2)51.51 (s, 9H), 1.70 (s,9H), 2.51 (s, 3H), 5.44 (s,
1H), 7.37 (d, 2H, J=7.9 Hz), 7.23 (d, 2H, J=7.9 Hz);
13C-NMR (126 MHz, 1:1 CDCl3–CS2) l 21.61 (q),
24.70 (s), 24.71 (s), 32.24 (q), 32.34 (q), 49.54 (d, 1C),
62.37 (s, 1C), 128.43 (d), 128.91 (s), 136.39 (s, 1C),
137.55 (d), 138.23 (s, 1C), 138.41 (s, 1C), 138.66 (s, 1C),
139.92 (s), 140.85 (s, 1C), 141.82 (s, 2C), 141.86 (s, 1C),
142.02 (s, 1C), 142.16 (s, 1C), 142.36 (s, 1C), 142.38 (s,
1C), 142.72 (s, 1C), 142.90 (s, 1C), 143.04 (s, 1C),
143.06 (s, 1C), 143.14 (s, 1C), 143.16 (s, 1C), 143.18 (s,
1C), 143.25 (s, 1C), 143.50 (s, 1C), 143.76 (s, 2C),
143.89 (s, 1C), 144.17 (s, 1C), 144.34 (s, 2C), 144.38 (s,
1C), 144.45 (s, 1C), 144.55 (s, 2C), 144.60 (s, IC),
144.89 (s, 2C), 145.04 (s, 1C), 145.13 (s, 1C), 145.22 (s,
1C), 145.33 (s, 1C), 145.53 (s, 2C), 146.28 (s, 2C),
146.65 (s, 1C), 146.92 (s, 1C), 146.97 (s, 1C), 147.03 (s,
1C), 147.18 (s, 1C), 147.48 (s, 1C), 147.69 (s, 1C),
148.29 (s, 1C), 148.48 (s, 1C), 148.80 (s, 1C), 148.93 (s,
1C), 150.06 (s, 1C), 150.08 (s, 1C), 151.82 (s, 1C),
157.16 (s, 1C), 161.84 (s, 1C);29Si-NMR(60 MHz, 1:1
CDCl3–CS2) 33.59; FAB MS 954–957(M+ +1 clus-
ter); UV–vis (toluene) umax (nm): 436 (br).
3g: brown solid; H-NMR (500 MHz, 1:1 CDCl3–
CS2) l 1.43 (s, 9H), 2.35 (s, 3H), 2.36 (s, 3H), 7.12 (d,
2H, J=7.7 Hz), 7.17 (d, 2H, J=7.7 Hz), 7.83 (d, 2H,
J=7.7 Hz), 7.89 (d, 2H, J=7.7 Hz); 13C-NMR (126
MHz, 1:1 CDCl3–CS2) d 21.61 (q), 21.63 (q), 22.32 (s),
29.12 (q), 64.99 (s, 2C), 127.61 (s), 127.67 (s), 128.26
(d), 128.35 (d), 136.52 (s, 2C), 136.74 (s, 2C), 137.40 (d),
137.51 (d), 138.68 (s, 2C), 139.59 (s, 2C), 139.72 (s),
139.76 (s), 140.55 (s, 2C), 141.30 (s, 2C), 141.47 (s, 2C),
142.07 (s, 2C), 142.14 (s, 2C), 142.34 (s, 2C), 143.36 (s,
2C), 143.80 (s, 2C), 144.29 (s, 2C), 145.44 (s, 2C),
145.86 (s, 2C), 145.88 (s, 4C), 146.01 (s, 2C), 146.06 (s,
2C), 146.40 (s, 2C), 146.81 (s, 2C), 146.93 (s, 2C),
147.00 (s, 2C), 147.74 (s, 2C), 148.55 (s, 2C), 150.22 (s,
2C), 152.90 (s, 2C), 162.39 (s, 2C), 164.07 (s, 2C);
29Si-NMR (80 MHz, 1:1 CDCI3CS2) 6–3.71; FAB
MA 1255–1257 (M+ +1 cluster).
1
4g: brown solid; H-NMR (500 MHz, 1:1 CDCl3–
CS2) l 1.44 (s, 9H), 2.47 (s, 6H), 7 31 (d, 2H, J=7.9
Hz), 7.33 (d, 2H, J=7.9 Hz), 7.95 (d, 2H, J=7.9 Hz),
8.09 (d, 2H, J=7.9 Hz); 13C-NMR (126 MHz, 1:1
CDCl3–CS2) 621.71 (q, two carbon), 22.74 (s), 29.31
(q), 49.06 (d, 1C), 61.27 (s, 1C), 127.03 (s), 127.45 (s),
128.55 (d), 136.42 (s, 1C), 137.93 (d), 138.05 (d), 138.09
(s, 1C), 138.16 (s, 1C), 138.33 (s, 1C), 138.49 (s), 139.90
(s, 1C), 140.12 (s), 140.15 (s), 140.85 (s, 1C), 141.62 (s,
1C), 141.66 (s, 1C), 141.92 (s, 1C), 141.95 (s, 1C),
142.24 (s, 1C), 142.34 (s, 1C), 142.51 (s, 1C), 142.70 (s,
2C), 142.84 (s, 1C), 142.94 (s, 1C), 142.98 (s, 2C),
143.07 (s, 1C), 143.08 (s, 1C), 143.13 (s, 1C), 143.21(s,
1C), 143.73 (s, 1C), 144.05 (s, 1C), 144.07(s, 1C), 144.21
(s, 1C), 144.30 (s, 1C), 144.33 (s, 1C), 144.37 (s, 1C),
144.39 (s, 1C), 144.46 (s, 1C), 144.55 (s, 2C), 144.82(s,
2C), 144.99(s, 1C), 145.16(s, 1C), 145.30(s, 1C), 145.41
(s, 1C), 145.51 (s, 1C), 146.33 (s, 1C), 146.62 (s, 1C),
146.64 (s, 1C), 146.98 (s, 2C), 147.13 (s, 1C), 147.49 (s,
1C), 147.68 (s, 1C), 148.19 (s, 1C), 148.48 (s, 1C),
148.65 (s, 1C), 148.95 (s, 1C), 149.90 (s, 1C), 153.18 (s,
1C), 151.01 (s, 1C), 157.59 (s, 1C), 161.31 (s, 1C);
29Si-NMR (80 MHz, 1:1 CDCl3–CS2) l −3.56; FAB
MS 989–991 (M+ +1 cluster); UV–vis (toluene) umax
(nm): 440 (br).
1
5f: brown solid; H-NMR (500 MHz, 1:1 CDCl3–
CS2) l 1.41 (s, 9H), 1.69 (s, 9H), 2.55 (s, 3H), 7.49 (d,
2H, J=7.9 Hz), 8.17 (d, 2H, J=7.9 Hz); 13C-NMR
(126 MHz, 1:1 CDCl3–CS2) 621.48 (q), 24.57 (s), 24.86
(s), 31.97 (q), 32.12 (q), 62.19 (s, 1C), 75.49 (s, 1C),
127.68 (s), 128.89 (d), 136.93 (s, 1C), 137.22 (s, 1C),
137.61 (s, 1C), 137.61 (d), 138.93 (s, 1C), 140.56 (s, 1C),
140.62 (s, 1C), 140.79 (s, 1C), 141.06 (s), 141.91 (s, 1C),
141.97 (s, 1C), 142.07 (s, 2C), 142.14 (s, 1C), 142.17 (s,
1C), 142.32 (s, 1C), 142.35 (s, 1C), 142.48 (s, 2C),
142.75 (s, 1C), 142.79 (s, 1C), 142.93 (s, 1C), 142.99 (s,
1C), 143.10 (s, 1C), 143.17 (s, 1C), 143.32 (s, 1C),
143.40 (s, 1C), 143.45 (s, 1C), 143.48 (s, 1C), 143.67(s,
1C), 143.73(s, 1C), 144.06 (s, 1C), 144.09 (s, 1C), 144.14
(s, 1C), 144.26 (s, 1C), 144.36 (s, 1C), 144.45 (s, 1C),
1
5g: brown solid; H-NMR (500 MHz, 1:1 CDCl3–
CS2) l 1.37 (s, 9H), 2.45 (s, 3H), 2.47 (s, 3H), 7.35 (d,
2H, J=7.8 Hz), 7.38 (d, 2H, J=7.8 Hz), 7.90 (d, 2H,
J=7.8 Hz), 8.08 (d, 2H, J=7.8 Hz); 13C-NMR (126
MHz, 1:1 CDCl3–CS2) d 21.59 (q), 21.63 (q), 22.17 (s),
29.45 (q), 61.93 (s, 1C), 75.94 (s, 1C), 126.69 (s), 127.03
Scheme 2.