264
L. Bereczki et al. / Tetrahedron: Asymmetry 18 (2007) 260–264
3
˚
heating. The crystallization was started by scraping the re-
cipient with a glass stick. The solution was cooled down
and left at room temperature for one week. The crystalline
final difference map was 0.15 and ꢀ0.15 e/A . The applied
2
2
o
2
weighting scheme was w ¼ 1=½r ðF Þ þ ð0:0179PÞ þ
2
2
0:4161Pꢂ where P ¼ ðF þ 2F Þ=3. Hydrogen atomic posi-
o
c
3
phase was filtered out and washed with water (2 · 0.5 cm )
tions were found on the difference Fourier maps.
to give 0.417 g of a crystalline product (26.1%). This was
3
dissolved in water (0.6 cm ) under heating after which cc.
Crystallographic data (excluding structure factors) for the
above crystal structure have been deposited with the Cam-
bridge Crystallographic Data Centre as supplementary
publication number CCDC 627510.
3
HCl (0.6 cm ) was added, and the solution cooled down
in a refrigerator. After 1 h, the solution was filtered and
3
washed with water (3 · 0.5 cm ). The process yielded
2
D
0
0
.286 g (S)-(+)-1, ½aꢂ = +48.8 (c 2, ethanol).
Acknowledgements
4
.4. X-ray crystallography
The Hungarian OTKA Foundation (Project Nos. T042725,
F037814 and T042642) and a diffractometer purchase grant
from the National Office for Research and Technology
Single crystals of (S)-1–(S)-2 were gained by salt formation
from (S)-(ꢀ)-1-phenylethylamine and (S)-(+)-N-formyl-
phenylalanine in water. A crystal of (S)-2–(S)-1 salt was
mounted on a loop.
(MU-00338/2003) are gratefully acknowledged for finan-
cial support.
Cell parameters were determined by least-squares of the
setting angles of 2693 reflections. Empirical formula:
C H10NO3 C H12N , formula weight: 314.38, colourless,
10 8
References
ꢀ
þ
needle crystals, size: 0.40 · 0.20 · 0.20 mm, crystal system:
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4
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´
8
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1
6
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1
1
1
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