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Application of spin labeling to drug assays. I. Synthesis of 2,2,6,6-tetramethylpiperidin-4-one-1-oxyl-15N-d16

✍ Scribed by Yul Yost; Carl F. Polnaszek; Ronald P. Mason; Jordan L. Holtzman

Publisher: John Wiley and Sons
Year: 1981
Tongue: French
Weight: 370 KB
Volume: 18
Category: Article
ISSN: 0022-2135
DOI: 10.1002/jlcr.2580180802

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✦ Synopsis

Spin l a b e l e d drugs can be u t i l i z e d f o r innnunoassays and determining t h e f r a c t i o n o f f r e e drug i n serum. To improve t h e sensit i v i t y we have synthesized t r i a c e t ~n a m i n e -~~N -d ~? by c y c l i z a t i o n o f phorone-d14 w i t h l5ND,. Phorone-d was obtained by condensat i o n o f acetone-d6. Triacetonamine-15N-d17 gave Temp0ne-~'N-d16, a n i t r o x i d e w i t h j u s t two absorption peaks on t h e ESR spectrum, whereas Tempone gives 3 peaks. The c o n t r i b u t i o n t o l i n e w i d t h o f methyl ene and methyl hydrogens o f Tempone i s eval uated by approp r i a t e s u b s t i t u t i o n o f p r o t i u m w i t h deuterium.

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