Table 2.
Entry | Compound | Vial methoda | “In-loop” methodb | RCP (%)e | Synthesis time (min) | Radioactivity at EOS (GBq (mCi))f | Molar radioactivity (GBq/μmol)g |
---|---|---|---|---|---|---|---|
| |||||||
RCY(%)c, d | RCY(%)c, d | ||||||
1 | [11C]2 | 33 | 70 (43)h | >99 | 35 | 10.2±2.8 (276±74) | 134±21 |
2 | [11C]5 | 5 | 72 (54)h | >99 | 33 | 14.3 (387) | 84 |
3 | [11C]7 | 2 | 30 (18)h | >99 | 38 | 3.8 (102) | 80 |
Conditions for vial reaction. (1) Precursor 1 (0.6 μmol); primary amines 3 and 6 (110 and 150 μmol, respectively); BEMP (5 μL, 34.6 μmol), DMF (80 μL); (2) 0.2% POCl3 (v/v) in MeCN (100 μL, 1.1 μmol); (3) secondary amine (4) in DMF (100 μL).
Conditions for “in-loop” reaction. (1) Precursor 1 (0.3 μmol); primary amines 3 and 6 (55 and 75 μmol, respectively); BEMP (2.5 μL, 17.3 μmol), DMF (40 μL); (2) 0.2% POCl3 (v/v) in MeCN (100 μL, 1.1 μmol); (3) secondary amine (4) in DMF (50 μL).
Non-isolated radiochemical yield (RCY), based on radio-HPLC analysis of the crude product.
Experiments were performed once (n=1).
Radiochemical purity (RCP) of the isolated product.
Total amount of the isolated product at the end-of-synthesis.
Molar radioactivity of the isolated product established by HPLC.
The decay-corrected radiochemical yield of the isolated product obtained after semi-preparative HPLC and formulation.