Tritium and deuterium labelling studies of alkali metal borohydrides and their application to simple reductions

被引：0

作者：

Than, C ^{[1
]}

Morimoto, H ^{[1
]}

Andres, H ^{[1
]}

Williams, PG ^{[1
]}

机构：

[1] SANDOZ PHARMA LTD,CHEM RES & DEV,CH-4002 BASEL,SWITZERLAND

来源：

JOURNAL OF LABELLED COMPOUNDS & RADIOPHARMACEUTICALS | 1996年 / 38卷 / 08期

关键词：

lithium borohydride; sodium borohydride; potassium borohydride; tritiated borane; boron NMR; tritium NMR; deuterium NMR;

D O I：

10.1002/(SICI)1099-1344(199608)38:8<693::AID-JLCR883>3.0.CO;2-4

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

Simple and facile syntheses of highly deuterated and tritiated LiBH4, NaBH4 and KBH4 were achieved by hydrogen isotope exchange with deuterium or tritium gas at elevated temperatures. The exchange products were characterized by boron, proton and deuterium or tritium NMR spectroscopy. The extent of isotope (H-2 or H-3) incorporation was calculated from the patterns of B-11 NMR spectra. Several samples of tritiated NaBH4 were treated with BF3-Et(2)O to produce tritiated borane-THF complex, which is an electrophilic reducing agent. The utility of both the borohydride reagents and borane-THF complex in labelling reactions was confirmed by exemplary reductions leading to specifically labelled products. The extent and orientation of labelling in the reduction products was assessed by a combination of radio-HPLC analysis, H-1, H-2 or H-3 NMR and mass spectrometry.

引用

页码：693 / 711

页数：19