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X. L. CUI ET AL.
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Synthesis of Tb(FBOPTPP)OH
The mixture of FBOPTPP (0.3 g, 0.40 mmol) and
.
TbCl3 6H2O (300 mg, 0.82 mmol) in imidazole (10 g) was
solvents for the characterisation of coordination compounds.
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heated at 2108C under the protection of dry N2 for about 2 h.
The extent of the reaction was followed by measuring the
UV-Vis spectra of the solution at 10-minute intervals. After
the reaction, the mixture was cooled to 1008C. Then, 100 mL
of chloroform was added, and then the mixture was extracted
by 200 mL distilled water. The topper solution was tested
with 0.1% aqueous AgNO3 until no AgCl precipitated.
The lower solution was purified by a neutral aluminum oxide
column (1.5 ꢀ 15 cm). The first band containing unreacted
FBOPTPP was eluted with chloroform containing 10%
ethanol. The second band was eluted with dimethylsulphoxide.
Dimethylsulphoxide in the eluant was removed under
reduced pressure, and the product about (0.12 g) was dried
in vacuo.
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Synthesis of Tb(FBOPTPP)acac
Tb(FBOPTPP)acac was prepared by the reaction of
.
Tb(acac)3 3H2O (0.5 g, 1.13 mmol) with FBOPTPP (0.2 g,
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0.27 mmol) in melting imidazole (10 g) at 2108C under the pro-
tection of dry N2 for about 3.5 h. The extent of the reaction was
followed by measuring the UV-Vis spectra of the solution. The
reaction mixture was cooled to 708C and 10 mL of ethanol was
added. Further, 20 mL of chloroform was added, and the
solution was extracted by distilled water. The crude product
was chromatographed on a neutral aluminum oxide column
(1.5 ꢀ 15 cm). The first band containing unreacted FBOPTPP
was eluted with chloroform containing 10% ethanol. The
second band was eluted with dimethylsulphoxide containing
50% ethanol. Water was added to the second fraction, and
the product was extracted by chloroform. The chloroform
fraction was concentrated and dried under vacuo, and the
yield this time through was about 0.1 g.
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Xiao, Ling Cui
