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Protecting groups in the preparation of thiolate complexes of technetium

Journal Article · · Inorganic Chemistry; (USA)
DOI:https://doi.org/10.1021/ic00341a019· OSTI ID:6128224
; ; ;  [1];  [2]
  1. Massachusetts Institute of Technology, Cambridge (USA)
  2. Harvard Medical School, Boston, MA (USA)
The nitrogen-sulfur ligand H{sub 2}PIC(Acm) (N-(2-((2- (((acetylamino) methyl)thio) acetyl) amino) ethyl)- 2-pyridinecarboxamide) reacted with (Bu{sub 4}N)(TcOCl{sub 4}) in methanolic solution, yielding the neutral complex (TcO(PIC)) (oxo(N- (2-((2- mercaptoacetyl) amino) ethyl)- 2-pyridine carboxamido) technetium(V)) as a red crystalline solid. The thiol-protected derivatives H{sub 2}PIC(Bzm) (Bzm = (benzoylamino) methyl) and H{sub 2}PIC(Bzl) (Bzl = benzyl) similarly gave (TcO(PIC)) in near-quantitative yield. In contrast, reaction of the unprotected, free-thiol form of the ligand, H{sub 3}PIC, with (Bu{sub 4}N)(TcOCl{sub 4}) in methanol gave a highly colored mixture of reduced technetium species and only traces of the neutral product. The ligand H{sub 2}PYR(Bzm) also reacted with (Bu{sub 4}N) (TcOCl{sub 4}) in methanol, giving a red neutral complex (TcO(PYR)). The X-ray structure of (TcO(PIC)) was determined. Crystal data for (TcO(PIC)): (C{sub 10}H{sub 10}N{sub 3}O{sub 3}STc), tetragonal, MW = 349.27, a = 8.010 (0) {angstrom}, c = 36.845 (0) {angstrom}, space group = P4{sub 3}2{sub 1}2, Z = 8, R = 0.037, R{sub w} = 0.041. 19 refs., 1 fig., 4 tabs.
OSTI ID:
6128224
Journal Information:
Inorganic Chemistry; (USA), Journal Name: Inorganic Chemistry; (USA) Vol. 29:16; ISSN 0020-1669; ISSN INOCA
Country of Publication:
United States
Language:
English