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Tritium labeling of 3 - trifluoromethyl - 4 - nitrophenol

✍ Scribed by John J. Lech; Phillip Moyer


Book ID
102368679
Publisher
John Wiley and Sons
Year
1972
Tongue
French
Weight
185 KB
Volume
8
Category
Article
ISSN
0022-2135

No coin nor oath required. For personal study only.

✦ Synopsis


EXPERIMENTAL

Reagents. Purified (98+%) 3-trifluoromethyl-4-nitrophenol was obtained from Farbwerke Hoechst Co., Bridgewater, New Jersey and was r e c r y s t a l l i z e d from benzene before use. Precoated s i l i c a g e l t h i n l a y e r chromatography p l a t e s ( s i lp l a t e -254) were obtained from t h e Brinkman Instrument Co., Westbury, L. I . , N. Y . . Prepacked s i l i c a g e l columns (Type D-32) were obtained from Quantum Ind u s t r i e s , F a i r f i e l d , N. J . . S c i n t i l l a t i o n counting materials were purchased from Packard I n s t . Co., Chicago, Ill., 3-methyl-4-nitrophenol and b n i t r o p h e n o l were obtained from Aldrich Chemical Co., Milwaukee, Wis.. solvents were of a n a l y t i c a l q u a l i t y .

Other chemicals and Procedure. TRITIATION. 0 . 5 gm of 3-trifluoromethyl-4-nitropheno1, mp 75-76O, was supplied t o Amersham-Searle Co., Arlington Heights, I l l . , f o r t r i t i u m labeling by Method TR-1 ( 3 ) . num c a t a l y s t and 100 C i of t r i t i a t e d water.

f o r f i v e hours. d u c t ( s ) was dissolved i n benzene and s e a l e d i n g l a s s ampules under nitrogen.

I n b r i e f , t h e TFM was mixed with 0.2 gm reduced p l a t i -

The mixture w a s heated t o 100Β°C After removal of l a b i l e tritium with ethanol t h e r e a c t i o n pro-*This p r o j e c t was supported i n p a r t by a Grant i n Aid by t h e Great Lakes Fishery Commission and by Sea Grant #I-35353 from t h e Department of Commerce.


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## Abstract Deuteration of p‐aminobenzoic acid hydrochloride (PABΒ·HCl) was studied to provide a model for tritiating PAB‐HCl. Tritium labeled PABΒ·HCl was used as the starting material for the synthesis of tritium labeled 1‐methyl‐4‐[4‐(7‐trifluoromethyl‐4‐quinolyl)aminobenzoyl]piperazine (Ic) and t