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Optimization of the Production of Lactam 2a
| |||||
|---|---|---|---|---|---|
| entry | scale (mg) | time (h) | temp | methoda | 2a:2b/cb |
| 1 | 200 | 16 | rt | vial | 1:0.95 |
| 2 | <5 | 1 | rt | vial | 1:1.1 |
| 3 | 23 | 0.75 | rt | slide | 1:0.56 |
| 4 | 100 | 4 | ~−78 °C | slide with N2 stream | 1:0.22 |
| 5 | 200 | 5 | ~−78 °C | slide with N2 stream | 1:0.24 |
Vial reactions run under a N2 atmosphere.
Ratios determined by 1H NMR analysis of the crude reaction mixture.
