3'(,3")-(二)甲酰基(二)苯并冠醚的2D NMR研究

2D NMR STUDY OF 3'(,3") -(di) -FORMYL-(di)-BENZO CROWN ETHERS

测定了3＇(, 3＂)-(二)甲酰基(二)苯并冠醚(1～7)的~1H、^(13)C谱,首次结合~1H-~1HCOSY、^(13)C-~1H COSY、COLOC二维谱对这些化合物的~1H、^(13)C化学位移进行了归属。用NOESY谱确定了合成产物冠4、冠5的结构,并对溶液中的构象异构体及其溶剂影响进行了初探。作者以冠1～8的~1H、^(13)C谱的归属为参照,提出了正确归属冠醚醚环上次甲基~1H、^(13)C化学位移的一般规则。

1H and 13C NMR spectra of 3'(, 3') -(di) -formyl-(di) -benzo crown ethers ( 1 ~7) and 4 '-formyl-benzo-15-crown-5(8) were recorded and assigned firstly by combination of 1H-1H COSY, 13C-1H COSY and COLOC 2D NMR experiments. The structures of Crown 4 and Crown 5 -the synthetic products were determined by 1H-1H NOESY spectra and rudimentary discussion was given for the conformational isomers of Crown 4. Referred to the 1H, 13C chemical shifts of Crown 1 ~ 8a general rule is proposed for the assignment of 1H, 13C chemical shifts of the methylenes of benzo crown ethers.