4114
H. Quan et al. / Tetrahedron 57 ꢀ2001) 4111±4114
1H NMR: d )ppm) 3.80 )s, 3H); 19F NMR: d )ppm) 274.56
)t,1F, J6.10); d )ppm) 269.43 )d,2F, J6.10).
Department Organization) of Japan. Thanks are also given
to Dr Zhi-heng Wu for his help in measuring XPS.
4.4. Reaction of 1 with 3
References
3 was prepared by the following procedure: around 100 g of
AlF3´3H2O was treated under different temperatures
between 208C and 7008C and kept for 10 h at the same
temperature )see Table 1). About 1.2 g of 3 was measured
and it was placed in an 80 cm3 stainless steel reactor, then
2.5 mmol of 1 was transferred into the reactor using vacuum
line. The reactor was heated to 2008C and kept for 1h under
stirring. The products were transferred to a trap )21968C)
and separated by trap-to-trap distillation )2908C and
21968C), and their amount and molecular weight were
measured. Then main products were analyzed by FT-IR,
GC-MS and 1H NMR and 19F NMR. The results are
shown in Table 1. The spectra data of 2 were listed as
follows; IR: 2969 )w); 1801)vs); 1449 )m); 1314 s; 1191
)vs); 1132 )vs); 1006 )s); 946 )s). MS peaks m/e: 15 1CH3;
50 1CF2; 59 1CH3CO; 85 1CF2Cl; 109 1CH3COCF2; 1 25
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1
1CH3COCFCl; 159 1CH2OCOCF2Cl. H NMR: d )ppm)
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2980 )w); 1888 )vs); 1273 )m); 1193 )s); 1106 )vs); 1028
)w); 969 )s). 19F NMR: d )ppm) 11.45 )s,1F); F2)2) d
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Acknowledgements
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We gratefully acknowledge the support of this investi-
gation by NEDO )New Energy and Industrial Technology
È
È
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