|
1. Azeotropic drying
|
|
K2.2.2.
|
12–15 mg
|
7.2 mg in 715 μL ACN
|
7.2 mg in 715 μL ACN
|
|
K2CO3
|
1 mL of a 1.0/mL solution
|
3.8 mg in 285 μL H2O
|
3.8 mg in 285 μL H2O
|
|
Evaporation/Temperature
|
145–150 °C 10 min
|
70–100 °C 10 min
|
95 °C 10 min
|
|
2. Radiofluorination
|
|
Precursor
|
3.5–4.5 mg
|
3 mg
|
5.5–6 mg
|
|
DMSO
|
0.6 mL
|
1 mL
|
0.8 mL
|
|
Reaction time
|
10 min
|
10 min
|
7 min 30
|
|
Temperature
|
165 °C
|
165 °C
|
155 °C
|
|
3. HPLC Purification
|
|
Eluent
|
H2O/CH3CN/TFA: 72/28/0.1
|
AcNH4 (0.1 M)/ CH3CN: 40/60
|
AcNH4 (0.1 M)/ CH3CN: 40/60 + Na-Asc (0.5%).
|
|
Flow rate
|
5 mL/min
|
4 mL/min
|
4 mL/min
|
|
Column
|
Symmetry®C18, Waters (300 × 7.8 mm, 7 μm)
|
Alltima® C18, Grace (250 X 10 mm, 5 μm)
|
Agilent Zorbax Eclipse XDB-C18 (250 X 9.4 mm, 5 μm)
|
|
4. Formulation
|
|
ETOH
|
2.0 mL
|
1.5 mL
|
2.5 mL
|
|
NaCl (0.9%)
|
8.0 mL (volume adjusted bring EtOH concentration below 10%)
|
13.5 mL
|
22.5 mL + Na-Asc (0.5%).
|
|
Synthetic results
|
|
Starting activity (GBq)
|
37
|
77.2 ± 2.1
|
102.7 ± 19
|
|
Radioactivity at EOS (GBq)
|
3.7–5.92
|
16.8 ± 1.9
|
23.8 ± 7.1
|
|
Radiochemical yield at EOS (%)
|
17.3–27.7
|
35.3 ± 5.1
|
32.7 ± 5.9
|
|
Activity yield at EOS (GBq)
|
10–16
|
23.3 ± 4.3
|
23.1 ± 4.5
|
|
Radiochemical purity (EOS)
|
> 95
|
99.4 ± 0.2
|
98.3 ± 0.5
|
|
Total synthesis time (min)
|
85–90
|
65.8 ± 3.8
|
48 ± 1.9
|
|
Molar activity at EOS(GBq/μmol)
|
37–111
|
158.6 ± 79.8
|
154.3 ± 51.1
|
