168
E. Lork et al. / Journal of Fluorine Chemistry 115 (2002) 165±168
1
À196 8C, and the l-tube was placed into a cryostat at
À40 8C for crystal growth. The air-sensitive salt 4 was
obtained as transparent orange-yellow crystals (1.71 g;
95%) after removal of the solvents, melting point (sealed
capillary) 125±126 8C (decomposition). NMR d (CD3CN):
by comparison of its melting point and H NMR spectrum
with those of an authentic sample.
Acknowledgements
1H: 2.85 (18H, TAS ), 2.11 (6H), 1.91 (3H), 1.61 (6H); 13C:
38.28 (TAS ), 57.33, 44.66, 37.47, 30.73, 14N: 105, À70,
The authors are grateful to Mr. Peter Brackmann for
technical assistance, and the Deutsche Forschungsge-
meinschaft (Germany) and the Russian Foundation for Basic
Research (Russia) for joint ®nancial support of this work
(Project 436 RUS113/486/0-2 R). Novosibirsk authors also
thank RFBR for an access to the STN International data-
bases via STN Center at their Institute (grant 00-03-32721).
À321 (TAS ).
N-(Adamant-1-yl)-N0-(2,3,5,6-tetra¯uoropyrid-4-yl) sulfur
diimide 6: A solution of 1.34 g (0.005 mol) of 2 and 0.85 g
(0.005 mol) of C5F5N in 5 ml of MeCN was added dropwise
to a stirred suspension of 0.76 g (0.005 mol) of freshly
calcinated CsF in 20 ml of MeCN under an argon atmo-
sphere at 20 8C. The reaction mixture was stirred overnight,
®ltered, the solvent was distilled off under reduced pressure,
and the residue was sublimed in vacuo and recrystallized
from hexane. Compound 6 was obtained as orange-yellow
crystals, melting point 59±60 8C, yield 1.47 g (85%). MS,
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