SYNTHESIS AND CHARACTERIZATION OF SOME POLYCYCLIC CYCLOBUTANONES
SYNTHESIS AND CHARACTERIZATION OF SOME POLYCYCLIC CYCLOBUTANONES
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DOI：
10.1021/jo00869a030
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发表时间：
1976-01-01
影响因子：
3.6
通讯作者：
MERRITT, VY
中科院分区：
文献类型：
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作者：
MILLER, RD;DOLCE, DL;MERRITT, VY
使用JEOL-PFT-100光谱仪结合EC-100 20 K存储计算机在25.03 MHz下以傅立叶模式测定碳-13光谱。该谱仪具有氘锁系统、JNM-SD-HC随机噪声（2500 Hz带宽）质子加速器和JNM-DP-1数字脉冲程序器。在加入5%MetSi作为内标的~ 0.5M氘代氯仿溶液（其也提供锁定信号）中测定化合物的光谱。所有样品均包含在精密研磨的10 mm OD管中。光谱仪用于交叉线圈配置。平均而言，使用了12 µ m脉冲，对应于大约45 °的倾斜角。对于5000 Hz的平均频谱宽度，脉冲之间的延迟为3 s。作者感谢美国国家科学基金会为格鲁吉亚大学化学系购买碳-13核磁共振光谱仪提供的相应资助。作者还感谢唐·K博士。打电话给考特尼·佩普先生，请他为这项工作提供技术援助。
Carbon-13 spectra were determined at 25.03 MHz in the Fourier mode using a JEOL-PFT-100 spectrometer in conjunction with an EC-100 20K memory computer. The spectrometer features a deu-terium locksystem, a JNM-SD-HC random noise (2500-Hz band-width) proton decoupler, and JNM-DP-1 digital pulse program-mer. Spectra of the compounds were determined in~ 0.5 M deuteriochloroform solution (which also provided the lock signal) with 5% MetSi added as internal reference. All samples were contained in precision ground 10 mm od tubes. The spectrometer was used in the crosscoil configuration. On the average, a 12-µß pulse, corre-sponding to an approximate tilt angle of 45, was employed. For the average spectral width of 5000 Hzthe delay between pulses was 3 s.Acknowledgment. The authors gratefully acknowledge a matching grant to the Chemistry Department, University of Georgia, from the National Science Foundation for pur-chase of the carbon-13 NMR spectrometer. The authors are also indebted to Dr. Don K. Dalling for helpful sugges-tions and to Mr. Courtney Pape for technical assistance in this work.