allowed to warm to ambient temperature. After stirring for
24 h, H2O2 aq. (30%, 4.5 mL) was added at 0 1C and the
resulting mixture was allowed to warm to ambient temperature
again. After stirring for 18 h, the reaction was quenched by the
addition of Na2SO3 aq. (10%, 50 mL) at 0 1C. After removal
of THF under reduced pressure, Na2SO3 aq. (10%, 150 mL)
was added and the organic layer separated. The aqueous layer
was extracted with CH2Cl2. The combined organic layer was
washed with water and brine, and dried over Na2SO4. After
concentration of the organic layer, the residual crude product
was purified by column chromatography (PSQ100B, 20/1
CH2Cl2/AcOEt, Rf = 0.27) to afford 1.57 g of 2 (3.0 mmol,
30% yield) as yellowish green solids: mp 192–193 1C. 1H NMR
(CDCl3, 400 MHz) d 2.26 (s, 3H), 2.70–2.82 (br, 6H),
6.88–6.90 (m, 6H), 7.04–7.17 (m, 16H). 31P{1H} NMR
(CDCl3, 162 MHz) d 50.60. HRMS calcd for C37H31OP:
522.2113. Found: 522.2115.
Commun., 2001, 1740; (b) H. Tong, Y. Dong, M. Haubler, J. W.
¨
Y. Lam, H. H.-Y. Sung, I. D. Williams, J. Sun and B. Z. Tang,
Chem. Commun., 2006, 1133; (c) H. Tong, Y. Hong, Y. Dong,
M. Haubler, J. W. Y. Lam, Z. Li, Z. Guo, Z. Guo and B. Z. Tang,
¨
Chem. Commun., 2006, 3705; (d) Y. Li, F. Li, H. Zhang, Z. Xie,
W. Xie, H. Xu, B. Li, F. Shen, L. Ye, M. Hanif, D. Ma and Y. Ma,
Chem. Commun., 2007, 231; (e) H. Tong, Y. Hong, Y. Dong,
Y. Ren, M. Haussler, J. W. Y. Lam, K. S. Wong and B. Z. Tang,
¨
J. Phys. Chem. B, 2007, 111, 2000; (f) Z. Zhao, Z. Wang, P. Lu, C.
Y. K. Chan, D. Liu, J. W. Y. Lam, H. H. Y. Sung, I. D. Williams,
Y. Ma and B. Z. Tang, Angew. Chem., Int. Ed., 2009, 48, 7608;
(g) J. Liu, J. W. Y. Lam and B. Z. Tang, J. Inorg. Organomet.
Polym., 2009, 19, 249.
6 G. Yu, S. Yin, Y. Liu, J. Chen, X. Xu, X. Sun, D. Ma, X. Zhan,
Q. Peng, Z. Shuai, B. Tang, D. Zhu, W. Fang and Y. Luo, J. Am.
Chem. Soc., 2005, 127, 6335.
7 (a) C.-H. Zhao, A. Wakamiya, Y. Inukai and S. Yamaguchi,
J. Am. Chem. Soc., 2006, 128, 15934; (b) A. Wakamiya, K. Mori
and S. Yamaguchi, Angew. Chem., Int. Ed., 2007, 46, 4273;
(c) M. Shimizu, Y. Takeda, M. Higashi and T. Hiyama, Angew.
Chem., Int. Ed., 2009, 48, 3653; (d) M. Shimizu, H. Tatsumi,
K. Mochida, K. Shimono and T. Hiyama, Chem.–Asian J., 2009,
4, 1289.
8 T. E. Kaiser, H. Wang, V. Stepanenko and F. Wurthner, Angew.
Chem., Int. Ed., 2007, 46, 5541.
9 (a) S. Yamaguchi and K. Tamao, Chem. Lett., 2005, 2;
´
(b) M. Hissler, P. Dyer and R. Reau, Coord. Chem. Rev., 2003,
244, 1; (c) A. Fukazawa and S. Yamaguchi, Chem.–Asian J., 2009,
4, 1386.
10 Representative reviews on phospholes: (a) A. N. Hughes and
C. Srivanavit, J. Heterocycl. Chem., 1970, 7, 1; (b) F. Mathey,
Chem. Rev., 1988, 88, 429; (c) L. D. Quin and A. N. Huges, in The
Chemistry of Organophosphorus Compounds, ed. F. R. Hartley,
¨
Notes and references
1 S. A. Jenekhe and J. A. Osaheni, Science, 1994, 265, 765.
2 (a) T. Sato, D.-L. Jiang and T. Aida, J. Am. Chem. Soc., 1999, 121,
10658; (b) J. M. Lupton, L. R. Hemingway, I. D. W. Samuel and
P. L. Burn, J. Mater. Chem., 2000, 10, 867; (c) L.-O. Palsson,
R. Beavington, M. J. Frampton, J. M. Lupton, S. W. Magennis, J.
P. J. Markham, J. N. G. Pillow, P. L. Burn and I. D. W. Samuel,
Macromolecules, 2002, 35, 7891; (d) Y.-H. Tseng, F.-I. Wu,
P.-I. Shih and C.-F. Shu, J. Polym. Sci., Part A: Polym. Chem.,
2005, 43, 5147; (e) T. Sanji, T. Kanzawa and M. Tanaka,
J. Organomet. Chem., 2007, 692, 5053; (f) J. Wang, Y. Zhao,
C. Dou, H. Sun, P. Xu, K. Ye, J. Zhang, S. Jiang, F. Li and
Y. Wang, J. Phys. Chem. B, 2007, 111, 5082.
Wiley, Chichester, 1990, vol. 1, pp. 295–384; (d) L. Nyula
´
Rev., 2001, 101, 1229; (e) M. Hissler, C. Lescop and R. Re
szi, Chem.
au, Pure
´
Appl. Chem., 2007, 79, 201; (f) Y. Matano and H. Imahori, Org.
Biomol. Chem., 2009, 7, 1258.
11 H.-C. Su, O. Fadhel, C.-J. Yang, T.-Y. Cho, C. Fave, M. Hissler,
3 Z. Xie, B. Yang, F. Li, G. Cheng, L. Liu, G. Yang, H. Xu, L. Ye,
M. Hanif, S. Liu, D. Ma and Y. Ma, J. Am. Chem. Soc., 2005, 127,
14152.
C.-C. Wu and R. Reau, J. Am. Chem. Soc., 2006, 128, 983.
´
12 (a) T. Sanji, K. Shiraishi and M. Tanaka, Org. Lett., 2007, 9, 3611;
(b) K. Shiraishi, T. Kashiwabara, T. Sanji and M. Tanaka, New J.
Chem., 2009, 33, 1680.
13 (a) U. Bankwitz, H. Sohn, D. R. Powell and R. West,
J. Organomet. Chem., 1995, 499, C7; (b) H. T. Teunissen,
C. B. Hansen and F. Bickelhaupt, Phosphorus, Sulfur Silicon Relat.
Elem., 1996, 118, 309.
4 (a) B.-K. An, S.-K. Kwon, S.-D. Jung and S. Y. Park, J. Am.
Chem. Soc., 2002, 124, 14410; (b) B.-K. An, D.-S. Lee, J.-S. Lee,
Y.-S. Park, H.-S. Song and S. Y. Park, J. Am. Chem. Soc., 2004,
126, 10232; (c) S.-K. Li, B.-K. An, S. D. Jung, M.-A. Chung and
S. Y. Park, Angew. Chem., Int. Ed., 2004, 43, 6346; (d) S. Y. Ryu,
S. Kim, J. Seo, Y.-W. Kim, O.-H. Kwon, D.-J. Jang and
S. Y. Park, Chem. Commun., 2004, 70; (e) H. W. Chung,
H. Yang, B. Singh, H. Moon, B.-K. An, S. Y. Lee and
S. Y. Park, J. Mater. Chem., 2009, 19, 5920.
14 E. H. Braye, W. Hubel and I. Caplier, J. Am. Chem. Soc., 1961, 83,
4406.
¨
15 R. Katoh, K. Suzuki, A. Furube, M. Kotani and K. Tokumaru,
J. Phys. Chem. C, 2009, 113, 2961.
16 The FF in the thin film was reported. See ref. 6.
5 (a) J. Luo, Z. Xie, J. W. Y. Lam, L. Cheng, H. Chen, C. Qiu,
H. S. Kwok, X. Zhan, Y. Liu, D. Zhu and B. Z. Tang, Chem.
ꢁc
This journal is The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2010
1540 | New J. Chem., 2010, 34, 1537–1540