Phosphonium- and borate-bridged zwitterionic ladder stilbene and its extended analogues
Phosphonium- and borate-bridged zwitterionic ladder stilbene and its extended analogues
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DOI：
10.1002/anie.200801834
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发表时间：
2008-01-01
影响因子：
16.6
通讯作者：
Yamaguchi, Shigehiro
中科院分区：
文献类型：
--
作者：
Fukazawa, Aiko;Yamada, Hiroshi;Yamaguchi, Shigehiro
将军。熔点（mp）用Stanford Research Systems OptiMelt MPA100仪器测定。1H和13C NMR谱用JEOL a -400或AL-400 （1H 400 MHz, 13C 100 MHz）光谱仪在CDCl3或C6D6中测量。化学位移以δ ppm报告，使用CHCl3 （7.26 ppm）或C6HD5 （7.15 ppm）用于1H NMR，使用CDCl3 （77.00 ppm）或C6D6 （128.06 ppm）用于13C NMR作为内部标准。11B核磁共振波谱用JEOL a -400或AL-400 （11B为128 MHz）谱仪记录，31P波谱用JEOL AL-400 （31P为162 MHz）谱仪记录，分别用BF3·OEt2 （0.0 ppm）和H3PO4 （0.0 ppm）作为外标。质谱用JEOL JMS700测定。薄层色谱（TLC）在0.25 mm厚的硅胶60f -254（默克）包被的板上进行。柱层析采用中性硅胶PSQ 60B或PSQ 100B （Fuji Silysia Chemical）。根据文献制备了双（2-溴苯基）乙炔、[1]1,4 -二乙基- 2,5 -双（二甲基苯基）苯、[2]1-溴-2-（三甲基硅基）乙炔、[1]和双（3-溴-2-噻基）乙炔[3]。除另有说明外，所有反应均在氩气气氛下进行。干四氢呋喃是从关东化学公司购买的。
General. Melting points (mp) were determined with a Stanford Research Systems OptiMelt MPA100 instrument. 1H and 13C NMR spectra were measured with a JEOL A-400 or AL-400 (400 MHz for 1H, and 100 MHz for 13C) spectrometer in CDCl3 or C6D6. Chemical shifts are reported in δ ppm using CHCl3 (7.26 ppm) or C6HD5 (7.15 ppm) for 1H NMR and using CDCl3 (77.00 ppm) or C6D6 (128.06 ppm) for 13C NMR as an internal standard. 11B NMR spectra were recorded with a JEOL A-400 or AL-400 (128 MHz for 11B) spectrometer, and 31P NMR spectra with a JEOL AL-400 (162 MHz for 31P) spectrometer using using BF3· OEt2 (0.0 ppm) and H3PO4 (0.0 ppm) as an external standard, respectively. Mass spectra were measured with a JEOL JMS700. Thin layer chromatography (TLC) was performed on plates coated with 0.25 mm thickness of Silica Gel 60 F-254 (Merck). Column chromatography was performed using neutral silica gel PSQ 60B or PSQ 100B (Fuji Silysia Chemical). Bis (2-bromophenyl) acetylene,[1] 1, 4-diethynyl-2, 5-bis (dimesitylboryl) benzene,[2] 1-Bromo-2-(trimethylsilyl) ethynylbenzene,[1] and bis (3-bromo-2-thienyl) acetylene [3] were prepared according to the literatures. All reactions were performed under an argon atmosphere, unless stated otherwise. Dry THF was purchased from Kanto Chemicals.