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. 2022 Sep 8;12(39):25457–25464. doi: 10.1039/d2ra05291a

Optimization of amounts of (S)-3a and rac-5a.

Entry Amount of (S)-3a (mmol) Amount of rac-5 (mmol) δR/S)b (ppm)
1 0.0125 0.05 0.02
2 0.025 0.05 0.03
3 0.05 0.05 0.04
4 0.1 0.05 0.06
5 0.1 0.0125 0.06
6 0.1 0.025 0.06
7 0.1 0.1 0.06
a

In NMR tube, the CSA (S)-3a (0.0125–0.1 mmol) and rac-5 (0.0125–0.1 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.

b

Calculated from the 1H-NMR spectrum.