Optimization of molar ratio of (R)-4 and rac-8a.
| Entry | Amount of rac-8 (mmol) | (ΔδR/S)b (ppm) | ||
|---|---|---|---|---|
| CH̲ | Ar-CH̲3 | CH̲3 | ||
| 1 | 0.0125 | No resol. | 0.04 | 0.04 |
| 2 | 0.025 | No resol. | 0.05 | 0.05 |
| 3 | 0.05 | No resol. | 0.05 | 0.06 |
| 4 | 0.1 | 0.16 | 0.13 | 0.09 |
| 5 | 0.2 | 0.09 | 0.06 | 0.05 |
In NMR tube, the CSA (R)-4 (0.1 mmol) and rac-8 (0.0125–0.2 mmol) were dissolved in chloroform-d (0.6 mL) and after shaking the NMR tube for 30 seconds, 1H-NMR spectrum was recorded on a 400 MHz NMR spectrometer at 25 °C.
Calculated from the 1H-NMR spectrum.