CHEMISTRY OF SULFENIC ACIDS .6. STRUCTURE OF SIMPLE SULFENIC ACIDS GENERATED BY FLASH VACUUM PYROLYSIS
CHEMISTRY OF SULFENIC ACIDS .6. STRUCTURE OF SIMPLE SULFENIC ACIDS GENERATED BY FLASH VACUUM PYROLYSIS
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DOI：
10.1021/jo00214a043
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发表时间：
1985-01-01
影响因子：
3.6
通讯作者：
BILLMERS, RL
中科院分区：
文献类型：
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作者：
DAVIS, FA;BILLMERS, RL
一般方法在所有反应中常规使用干燥氮气作为气氛。所有玻璃器皿在使用前在110-120 ℃下烘烤至少1小时。熔点是未校正的，并且是用Hoover装置获得的。在Bruker Spectrospin Model AM 250或WM 250上获得约10%（w/v）的CDCl 3溶液的1H、13 C和31 P NMR。相对于作为内标的四甲基硅烷（用于31 P NMR的磷酸），化学位移以百万分率（5标度）报告。以下缩写已用于报告NMR数据：以赫兹计的偶合常数（J）;单峰（s）;双峰（d）;双峰的双峰（dd）;三重峰（t）;四重峰（q）;和多重峰（m）。在分辨率为3300或5000的Du蓬特21- 492 B仪器上记录精确的质谱。乙腈经氢化钙干燥并经P2 O 6蒸馏。在薄层色谱法中使用Eastman Chromagram（在聚乙烯上具有荧光指示剂的硅胶）预涂板。Baker硅胶（60-200目）和EM 774硅胶用于柱色谱。
General Methods. Dry nitrogen was routinely used as the atmosphere in all reactions. All glassware was baked at 110-120 C for at least 1 h before use. Melting points are uncorrected and were obtained with a Thomas-Hoover apparatus. The XH, 13C, and 31P NMR of approximately 10%(w/v) solutions in CDC13 were obtained on a Bruker Spectrospin Model AM 250 or WM 250. Chemical shifts are reported in parts per million (5 scale) vs. tetramethylsilane (phosphoric acid for 31P NMR) as an internal standard. The following abbreviations have been used in reporting NMR data: coupling constant in hertz (J); singlet (s); doublet (d); doublet of doublets (dd); triplet (t); quartet (q); and multiplet (m). Precise mass spectra were recorded on a Du Pont 21-492B instrument with a resolution of 3300 or 5000. Acetonitrile was dried over calcium hydride and distilled over P206. Eastman Chromagram (silica gel with fluorescent indicator on polyethylene) precoated sheets were used in thin-layer chromatography. Baker silica gel (60-200 mesh) and EM 774 silica gel for column chro-