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zhangwei章薇铁虫 (初入文坛)
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4-Dibutylaminobenzaldehyde. 1H NMR (500 MHz, CDCl3, δ): 9.67 (s, 1H), 7.66 (d, J ¼ 8.5 Hz, 2H), 6.61 (d, J ¼ 9 Hz, 2H), 3.32 (t, 4H), 1.41 (m, 8H), 0.84 (t, 6H). 4-Diheptylaminobenzaldehyde. 1H NMR (500 MHz, CDCl3,δ): 9.67 (s, 1H), 7.67 (d, J ¼ 8.5 Hz, 2H), 6.61 (d, 2H), 3.32 (t, 4H), 1.60 (m, 4H), 1.31 (m, 16H), 0.86 (t, 6H). 4-Dioctylaminobenzaldehyde. 1H NMR (500 MHz, CDCl3, δ):9.71 (s, 1H), 7.71 (d, J ¼ 7.5 Hz, 2H), 6.67 (d, 2H), 3.31 (t, 4H),1.61 (m, 4H), 1.32 (m, 20H), 0.91 (s, 6H). 4-Didecylaminobenzaldehyde. 1H NMR (500 MHz, CDCl3, δ):9.68 (s, 1H), 7.68 (d, J ¼ 8.5 Hz, 2H), 6.62 (d, J ¼ 9 Hz, 2H), 3.32(t, 4H), 1.55 (m, 4H), 1.26 (t, 28H), 0.87 (t, 6H). 4-Didodecylaminobenzaldehyde. 1H NMR (500 MHz, CDCl3,δ): 9.67 (s, 1H), 7.69 (d, J ¼ 9 Hz, 2H), 6.63 (d, J ¼ 9 Hz, 2H), 3.32(t, 4H), 1.57 (m, 4H), 1.28 (t, 36H), 0.85 (t, 6H). Synthesis of 2,6-bis(diethylphosphorylmethyl)-9,10-distyrylanthracene A pressure tube containing styrene (1.11 g, 10.1 mmol), 2,6-bis(diethylphosphorylmethyl)-9,10-dibromoanthracene (1.35g, 2.13 mmol), Pd(OAc)2 (52 mg, 0.21 mmol), tri(o-tolyl) phosphine (0.38 g, 1.21 mmol), N(C2H5)3 (7 mL) and THF (7mL) was sealed with a helix teflon cap under nitrogen and then refluxed at 80 C for 24 h. After cooling, the solvents were evaporated and the residue was separated by column chromatography on silica gel using ethyl acetate–hexane (3/1) as the eluent. Yield: 1.16 g (80.6%). 1H NMR (500 MHz, CDCl3, δ): 8.35 (d, J ¼ 9 Hz, 2H), 8.21 (s, 2H), 7.89 (d, J ¼ 11.5 Hz, 2H), 7.69 (d, J ¼ 7.5 Hz, 4H), 7.48 (m, 6H), 7.39 (m, 2H), 6.92 (d, J ¼17 Hz, 2H), 4.03 (m, 8H), 3.33 (d, 4H), 1.23 (m, 12H). Anal. calcd for C40H44O6P2: C, 70.37; H, 6.50; O, 14.06; P, 9.07. Found: C, 70.46; H, 6.44 |
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刁刁8888
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2楼2014-09-22 10:04:21
zhangwei章薇
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3楼2014-09-23 12:34:18
