Stereocontrolled creation of adjacent quaternary and tertiary stereocenters by a catalytic conjugate addition
Stereocontrolled creation of adjacent quaternary and tertiary stereocenters by a catalytic conjugate addition
复制标题
DOI：
10.1002/anie.200461923
复制
发表时间：
2005-01-01
影响因子：
16.6
通讯作者：
Deng, L
中科院分区：
文献类型：
--
作者：
Li, HM;Wang, Y;Deng, L
在瓦里安仪器（分别为400 MHz和100 MHz）上记录1H和13C核磁共振光谱，内部参考四甲基硅烷信号或残余比例溶剂信号。1H NMR数据记录如下：化学位移（δ, ppm），多重度（s，单重态；d，双重态；t，三重态；q，四重奏；m，多重态），耦合常数（Hz），积分。13C核磁共振数据以化学位移（δ, ppm）表示。在珀金-埃尔默红外光谱仪上记录了红外光谱，并报道了吸收频率。用20 eV、CH4/CI或NH3/CI测定的所有新化合物的低分辨率质谱在Hewlett-Packard 5989A GC/MS上记录，精确质谱在VG 7070高分辨率质谱仪上记录。在Jasco数字偏振计上测量了特定的旋转。高压液相色谱（HPLC）分析在配备四元泵的惠普1100系列仪器上进行，使用Daicel Chiralcel OJ， OD柱（250 x 4.6 mm）或Chiralpak AD柱（250 x 4.6 mm）。在220 nm或215 nm处进行紫外检测。本文所报道结构的晶体学数据（不包括结构因素）已作为补充出版物CCDC-249709 (5Ba), CCDC-249710 (5Dd), CCDC-249711 （5De）存放在剑桥晶体学数据中心。申请人可向CCDC（剑桥CB21EZ联合路12号）申请免费索取资料副本。英国(传真：（+ 44）1223-336-033；电子邮件：deposit@ ccdc。凸轮。ac.英国)。
General Information. 1H and 13C NMR spectra were recorded on a Varian instrument (400 MHz and 100 MHz, respectively) and internally referenced to tetramethylsilane signal or residual protio solvent signals. Data for 1H NMR are recorded as follows: chemical shift (δ, ppm), multiplicity (s, singlet; d, doublet; t, triplet; q, quartet; m, multiplet), coupling constant (Hz), intergration. Data for 13C NMR are reported in terms of chemical shift (δ, ppm). Infrared spectra were recorded on a Perkin Elmer FT-IR Spectrometer and are reported in frequency of absorption. Low resolution mass spectra for all the new compounds done by either 20 eV, CH4/CI or NH3/CI were recorded on a Hewlett-Packard 5989A GC/MS, and exact mass spectra on a VG 7070 high resolution mass spectrometer. Specific rotations were measured on a Jasco Digital Polarimeter. High pressure liquid chromatography (HPLC) analysis was performed on a Hewlett-Packard 1100 Series instrument equipped with a quaternary pump, using a Daicel Chiralcel OJ, OD Column (250 x 4.6 mm) or Chiralpak AD Column (250 x 4.6 mm). UV detection was monitored at 220 nm or at 215 nm.Crystallographic data (excluding structure factors) for the structures reported in this paper have been deposited with the Cambridge Crystallographic Data Center as supplementary publication nos. CCDC-249709 (5Ba), CCDC-249710 (5Dd), CCDC-249711 (5De). Copies of the data can be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB21EZ. UK(fax:(+ 44) 1223-336-033; e-mail: deposit@ ccdc. cam. ac. uk).