X. Chen et al. / Journal of Organometallic Chemistry 655 (2002) 89ꢁ
/95
95
(C6D6, 300 Hz): d 0.07(s, 9H, SiMe3), 0.49(s, 9H,
SiMe3), 1.16 (s, 9H, CMe3), 5.69 (s, 1H, CH) 7.54ꢁ
8.56 (m, 4H,pyridyl).
5. Supplementary material
/
Crystallographic data for the structures reported in
this paper have been deposited with the Cambridge
Crystallographic Data Centre, CCDC no. 151058 for
complex 1, no. 151057 for complex 7, no. 151059 for
complex 6 and no. 151056 for complex 10. Copies of this
information may be obtained free of charge from The
Director, CCDC, 12 Union Road, Cambridge CB2 1EZ,
ꢀ
ꢁ
/
4.7. [/
Li{N(R)C(But)C(H)C(p-pyridyl)N
R}]2 (8)
As same procedures for complex 7 thus p-Cyanopyr-
ꢀ
ꢁ
idine (0.81 g, 7.78 mmol) [ HR]2 (1.93 g,
LiN(R)C(But)C
/
/
UK (Fax: ꢂ44-1223-336033; e-mail: deposit@ccdc.ca-
/
7.78 mmol) in diethyl ether (ca. 25 cm3) gave yellow
precipitate (1.31 g, 48%, analyzed as 8), and the filtrate
was concentrated to get another part of crystalline
complex 8 (0.57 g, 21%), the total yield was 79%. H-
NMR (C6D6, 300 Hz): d 0.07 (s, 9H, SiMe3), 0.51 (s,
1
Acknowledgements
9H, SiMe3), 1.49 (s, 9H, CMe3), 5.49 (s, 1H, CH) 6.43ꢁ
8.56 (m, 4H, pyridyl).
/
This work was supported by Natural Science Foun-
dation of China (29872024 and 20171030, D.-S.L.) and
the Youth Science Foundation of Shanxi Province
(20001004, X.C.).
4.8. 2,4,-(bis)o-Pyridyl-6-tertbutyl-1,3,5-triazine (9)
o-Cyanopyridine (0.939 g, 9.01 mmol) was added to a
References
ꢀ
ꢁ
stirred solution of [ HR]2 (2.36 g, 9.49
LiN(R)C(But)C
/
/
mmol) in diethyl ether (ca. 20 cm3) at 0 8C for 30 min.
The mixyure was stirred for 12 h at r.t. and filtered. The
air-stable yellow preciptate of compound 9 was obtained
[1] P.B. Hitchcock, M.F. Lappert, D.S. Liu, J. Chem. Soc. Chem.
Commun. (1994) 2637.
[2] P.B. Hitchcock, M.F. Lappert, D.S. Liu, J. Chem. Soc. Chem.
Commun. (1994) 1699.
1
(0.52 g, 41%). H-NMR (C6D6, 300 Hz): d 1.33 (s, 9H,
6.99 (m, 2H, pyridyl), 7.30 (s, 1H, pyridyl),
8.88 (m, 2H, pyridyl) 9.50 (s,
[3] P.B. Hitchcock, M.F. Lappert, D.S. Liu, J. Organomet. Chem.
488 (1995) 241.
CMe3), 6.92ꢁ
/
[4] P.B. Hitchcock, M.F. Lappert, D.S. Liu, et al., J. Chem. Soc.
Dalton Trans. (1999) 1263.
8.17 (m, 1H, pyridyl), 8.72ꢁ
/
1H, pyridyl), 10.36 (s, 1H, pyridyl).
[5] P.C. Blake, M.A. Edelman, P.B. Hitchcock, J. Hu, M.F. Lappert,
S. Tian, G. Muller, J.L. Atwood, H.M. Zhang, J. Organomet.
Chem. 261 (1998) 270.
[6] P.B. Hitchcock, M.F. Lappert, M. Layh, D.S. Liu, R. Sablong, T.
Shun, J. Chem. Soc. Dalton Trans. (2000) 2301.
[7] P.L. Compagnon, M. Miocque, Ann. Chim. (France) 5 (1970) 23.
[8] R.M. Anker, A.H. Cook, J. Chem. Soc. (1941) 323.
[9] L.O. Moore, J. Org. Chem. 31 (1966) 3910.
[10] (a) D.J. Berry, B.J. Wakefield, J. Chem. Soc. C (1971) 642.;
(b) D.J. Berry, J.D. Cook, B.J. Wakefleld, J. Chem. Soc. Perkin I
(1972) 2190.
4.9. 2,4,-(bis)p-Pyridyl-6-tertbutyl-1,3,5-triazine (10)
p-Cyanopyridine (0.61 g, 6.48 mmol) was added to a
stirred solution of [LiN(R)C(But)CHR]2 (0.81 g, 3.24
mmol) in diethyl ether (ca. 20 cm3) at 0 8C for 30 min.
The mixture was stirred for 12 h at r.t. and filtered.
The air-stable precipitate of compound 10 was
obtained (0.72 g, 76%) and a suitable single crystal
was obtained by recrystallization in Et2O. (Found: C,
70.28; H, 6.12; N, 23.34, C17H117N5 requires C, 70.08;
H, 5.88; N, 24.04%.) 1H-NMR (CDC13, 300 Hz): d 1.73
[11] L.S. Cook, B.J. Wakefield, Tetrahedron Lett. (1976) 147.
[12] L.S. Cook, B.J. Wakefield, J. Chem. Soc. Perkin I (1980) 2392.
[13] J.H. Forsberg, V.T. Spaziano, J. Heterocyclic Chem. 25 (1988)
267.
[14] J.H. Forsberg, V.T. Spaziano, J. Org. Chem. 52 (1987) 1017.
[15] F. Xu, J.H. Sun, Q. Shen, The 19th IUPAC International
Conference on Organometallic Chemistry, July 2000, PS 182.
(s, 9H, CMe3), 8.02ꢁ9.08 (m, 8H5 pyridyl).
/