Table 2.
Entry | Zn form | Supplier | Conv. [%][a] | Yield [%][a] |
---|---|---|---|---|
1 | zinc granular, 20–30 mesh | Sigma–Aldrich | 97 | 81 |
2 | zinc granular, 20 mesh | Sigma–Aldrich | 99 | 72 |
3 | zinc foil, 0.25 mm thick, 99.9 % | Sigma–Aldrich | 99 | 77 |
4 | zinc dust, <10 mm | Sigma–Aldrich | 98 | 80 |
5 | zinc puriss, ACS reagent, >99.9 % | Sigma–Aldrich | 91 | 66 |
6 | zinc shot, 10 mm dia., 2 mm thick, 99.99 % |
Sigma–Aldrich | 87 | 53 |
7 | zinc flake, ca. 325 mesh, 99.9 % | Alfa Aesar | 99 | 87 |
8 | zinc wire, 0.04 in dia., 99.95 % | Alfa Aesar | 95 | 75 |
9 | zinc powder, 6–9 μm, 97.5 % | Alfa Aesar | 99 | 83 |
10 | zinc metal powder | Fisher Scientific | 98 | 68 |
11 | zinc, ≥99%, mossy | Acros | 96 | 73 |
12 | zinc foil, 0.38 mm | BDH chemicals | 99 | 73 |
Reaction conditions: benzaldehyde (1 mmol), ethyl 2‐bromoacetate (1.2 mmol), zinc form as specified (2 equiv), mixer mill, 30 Hz, 2 h. [a] Conversion and yield were determined by 1H NMR spectroscopy with mesitylene as an internal standard.