S. Dissoki et al.
[18F]FB-GE11′ ([18F]-1)
evaporated; and the remaining mixture was neutralized by the
addition of 1M NaOH, passed through an SPE C-18 cartridge,
washed with water (5mL), and eluted with ethanol (0.5mL).
To a solution of [18F]SFB in DMSO (0.2mL), 660mg of GE11′ in
DMSO was added, followed by the addition of DIPEA (10mL);
the mixture was stirred for 40min at 60ꢁC.32 The reaction mix-
ture was cooled, diluted with water/acetonitrile 50:50 (v/v), and
injected into an HPLC preparative column eluted with a mixture
of water/acetonitrile/0.1% TFA (80:20, v/v) (flow rate, 8mL/min).
The labeled product was collected (Rt=22min) and evaporated
to remove acetonitrile and TFA, and then neutralized by the
addition of 1M NaOH. The product solution was passed through
an SPE C-18 cartridge, washed with water (10mL), and eluted
with ethanol (0.3mL). [18F]-1 was obtained after a total radio-
synthesis time of 3.5h, with a DCY of 22%, a SA of 108Ci/mmol,
and 95% RCP (n=2).
[
18F]-3 was obtained after a total radiosynthesis time of 2.5h,
with a DCY of 10%, a SA of 500Ci/mmol and 98% RCP (n=2).
[
111In]NOTA- GE11′ ([111In]-4)
The precursor 11 (1mg, 0.42mmol) dissolved in 0.1mL of 0.1M
ammonium acetate buffer (pH5.5) was added to a solution
of [111In]InCl3 (0.5–2mCi). The mixture was heated to 50ꢁC for
1h,38 and the reaction was terminated by the addition of 10mL
of 10nM EDTA solution. The crude product was filtered and
injected into an HPLC preparative column eluted with a mixture
of water/acetonitrile/0.1% TFA (80:20, v/v) (flow rate, 8mL/min).
The collected fractions were combined (Rt=13.6min), and aceto-
nitrile/TFA were removed. The product solution was loaded on
an SPE C-18 cartridge and eluted with ethanol (0.5mL). The final
product, [111In]-4, was obtained after a total radiosynthesis time
of 2h, with a DCY of 60%, a SA of 0.35Ci/mmol, and 100% RCP
(n=2).
[
124I]Succinimidyl 4-iodobenzoate
Na124I solution (0.02M NaOH) was evaporated to dryness under
nitrogen stream, and 0.2mL of STB (1mg/mL in methanol) was
added followed by the addition of N-chlorosuccinimide (50mL,
1mg/mL in methanol) and 5% acetic acid (350mL, in methanol).25
The reaction mixture was stirred for 20min at RT, purified, and
eluted with acetonitrile (2mL) on an SPE C-18 Sep-Pak (Oasis)
to afford [124I]SIB with 65% RCY, a SA of 3600Ci/mmol, and
95% RCP (n=2).
References
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[
124I]IB-GE11′ ([124I]-2)
Triethylamine (50mL) and 2.5mg of GE11′ (5mg/mL in DMF) were
added to dried [124I]SIB. The reaction mixture was incubated for
1h at RT,33 diluted with water/acetonitrile 50:50 (v/v), and
injected into an HPLC preparative column eluted with a mix-
ture of water/acetonitrile 75: 25 (v/v) (flow rate, 8mL/min).
The collected fractions containing [124I]IB-GE11′ were com-
bined (Rt=26min) and evaporated to remove acetonitrile and
TFA, and then neutralized by the addition of 1M NaOH. The pro-
duct solution was passed through an SPE C-18 cartridge, washed
with water (4mL), and eluted with ethanol (0.5mL). [124I]-2 was
obtained after a total radiosynthesis time of 2.5h, with 30%
RCY, a SA of 300Ci/mmol, and 98% RCP (n=2).
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[18F]F-PEG4-propyne ([18F]-6)
A solution of 7 (5mg/mL in DMSO) was added to the reactor con-
taining the dried complex K18F/kryptofix. The solution was
heated to 110ꢁC for 10min,34 cooled to 35ꢁC, diluted with 1mL
of acetonitrile/water 50:50 (v/v), and injected into an HPLC pre-
parative column eluted with water/acetonitrile/0.2% TFA (70:30)
(v/v) (flow rate, 6mL/min). The labeled product was collected
(Rt=12min) in a flask diluted with water (50mL) and loaded onto
an SPE C-18 cartridge, washed with water (10mL), and eluted
with THF (2mL) to obtain [18F]-6 with a DCY of 30%, a SA of
2580Ci/mmol, and a RCP of 100% (n=5).
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[
18F]-6 in acetonitrile (0.3mL) was reacted with compound 10
(1mg, 0.0005mmol) in the presence of sodium ascorbate (32mg,
0.16mmol), CuI (3mg, 0.016mmol), DIPEA (30mL, 0.175mmol) in
a mixture of DMF (0.2mL) and water (0.25mL).36 The reaction
mixture was stirred vigorously at RT for 10min. The crude prod-
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preparative column eluted with a gradient of water/acetoni-
trile/0.2% TFA 85:15 (v/v) (flow rate, 8mL/min). The prod-
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Copyright © 2011 John Wiley & Sons, Ltd.
J. Label Compd. Radiopharm 2011, 54 693–701