Table 1.
No. | CD | Milling time [h] | B2M ratioa | Productb [g] | DSc | Yieldd [%] |
1 | β | 2 | 14.6 | 2.3 | 4.4 | 84 |
2 | β | 4 | 14.6 | 2.3 | 5.6 | 78 |
3 | β | 3.5 | 14.6 | 2.5 | 5.3 | 87 |
4 | β-hydrate | 3.5 | 13.0 | 2.4 | 3.7 | 89 |
5 | γ | 2 | 13.2 | 2.7 | 5.1 | 84 |
6 | γ-hydrate | 3.5 | 12.2 | 2.4 | 5.5 | 73 |
aBall-to-mass (mass of balls/mass of reagents); bisolated, purified; ccalculated from the integration of the anomeric-proton and CH3 signals of 1H NMR spectra and corrected using the residual solvent content; don the base of DS.