Table 4. Large-Scale Syntheses of 1 under Optimized Conditions (Step 2, Scheme 4).
| entry | scale (g) | HPLC IPC (area % at 245 nm) | isolated product | |||
|---|---|---|---|---|---|---|
| wt (g) | HPLC (area % at 245 nm) | purity (wt %) | yield (%) | |||
| 1 | 5 | 92.7 | 7.1 | 96.2 | 95.0 | 84 |
| 2 | 10 | 91.2 | 13.6 | 97.6 | 91.0 | 84 |
| 3 | 50 | 92.6 | 66.4 | 99.5 | 99.3 | 86 |
| 4 | 100 | 94.0 | 135 | 100 | 99.0 | 88 |