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zhangwei章薇鐵蟲 (初入文壇)
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[求助]
幫幫忙,翻一下,謝謝!
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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 |

鐵桿木蟲 (著名寫手)
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合成 2,6-bis(diethylphosphorylmethyl)-9,10-distyrylanthracene 高壓反應管內(nèi)加入苯乙烯 (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) ,氮氣保護下。螺旋特氟龍蓋密封。80度回流24小時,冷卻,溶劑蒸發(fā),殘留物硅膠柱層析分離提純, 洗脫液乙酸乙酯-正己烷(3:1)收率: 1.16 g (80.6%). 核磁數(shù)據(jù): 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). 元素分析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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