✍ Scribed by Y. W. Lee; E. E. Knaus; L. I. Wiebe
No coin nor oath required. For personal study only.
Reaction of 2,2^1^‐anhydrouridine (2) with [^82^Br]‐ammonium bromide in the presence of one equivalent p‐toluenesulfonic acid afforded 2^1^‐[^82^Br]‐2^1^‐deoxyuridine (3) in 73.4% chemical yield with a specific activity of 0.58 mCi mM^−1^. Alternatively, direct activation of 2^1^‐bromo‐2^1^‐deoxyuridine at a thermal neutron flux of 1 × 10^12^n cm^−2^s^−1^ gave 2^1^‐[^82^Br]‐2^1^‐deoxyuridine, with a specific activity of 0.6‐0.7 mCi mM^−1^ for a 3 hr irradiation. 2^1^‐[^82^Br]‐2^1^‐deoxyuridine was rapidly purified by high pressure liquid chromatography with an elution time of 18 minutes, or by preparative thin layer chromatography.
📜 SIMILAR VOLUMES
## Abstract The synthesis of [21‐^13^C]‐cholesterol (5) from 3β‐O‐(t‐butyldimethylsilyl)‐17β‐cyano‐androst‐5‐ene (1) is described. Labelled carbon‐atom was introduced by Grignard reaction of nitrile derivative with [^13^C]‐methylmagnesium iodide. Location of label was confirmed by ^13^C‐NMR spectro
pregnenolone using pregnenolone as s t a r t i n g m a t e r i a l i e described. The procedure involved r e m o v a l of t h e C-21-methyl group of t h e s t e r o i d and t h e side-chain w a s reconstructed with 3H -CH3MgI i n two steps: a Grignard reaction followed by oxidation of t h e resultin