| Overview |
| Instructions |
| Operating scheme |
| Substances |
| Equipment |
| Evaluation |
| Analytics |
| - Chromatogram |
| - 1H-NMR |
| - 13C-NMR |
| - IR |
| + |
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; Side reactions |
Chromatogram |
| HPLC: crude product | |
| column | Phenomenex Luna C18; particle diameter 3 µm, L= 150 mm, ID= 4.6 mm |
| column temperature | 25 °C |
| injection | 15 µL |
| mobile phase | gradient: 3% methanol/water --> 98% methanol/water in 30 min, 10 min isocratic |
| flow | 0.6 mL/min |
| detector (UV 220 nm) | percent concentration calculated from relative peak area |
| GC: pure product | |
| column | Zebron ZB-1, L=15 m, d=0.25 mm, film=0.25 µm |
| inlet | injector: 250°C, split injection, 0.2 µl |
| carrier gas | He, pre-column pressure 90 kPa |
| oven | 30°C (4 min), 20°C/min --> 240°C (7 min) |
| detector | FID, 230°C, H2 30.8 mL/min, synth. air 361 mL/min |
| integration | percent concentration calculated from relative peak area |