Table 4.
Radiosynthesis of methyl 4-bromobenzoate
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---|---|---|---|---|
Entry | Precursor (mg) | H2O (μL) | Solvent (500 μL) | Microwave (30 sec)
|
Yield (%) [Ratio]1 | ||||
1 | 5 | / | DMF | 70/23 |
2 | 2.5 | / | DMF | 69/232 |
3 | 0.5 | / | DMF | 70/18 |
4 | 2.5 | 50 | DMF | 64/25 |
5 | 2.5 | 100 | DMF | 63/19 |
6 | 2.5 | 1003 | DMF | 76/19 |
7 | 2.5 | / | DMSO | 75/22 |
8 | 4 | / | DMSO4 | 77/19 |
9 | 5 | / | DMF5 | 77/20 |
Notes:
Yield of methyl 4-bromobenzoate/bromobenzene by radioTLC and HPLC;
96% (+30 sec microwave), and 97% (+60 sec microwave);
With KBr (100 μg);
[6Br]bromide after 7 half-lives;
MQA method was used to elute radioactivity (0.5 mCi) with 8 in DMF (5×1 mg/0.1 mL) in 98% efficiency. Reaction condition: microwave 2×30 sec with interval of 30 sec.