Table 4.
Solvent screening for the acylation of (±)‐7 [a].
Entry | Solvent | ee s [b] [%] | ee p [b] [%] | Conv. [%] | E |
---|---|---|---|---|---|
1 | toluene | 20 | 99 | 17 | >200 |
2 | methyl tert‐butyl ether | 4 | 99 | 4 | >200 |
3 | acetonitrile | 1 | 95 | 1 | 39 |
4 | diisopropyl ether | 20 | 99 | 17 | >200 |
5 | chloroform | 2 | 73 | 3 | 7 |
6 | 1,4‐dioxane | 3 | 99 | 3 | >200 |
[a] Substrate (0.0125 mmol, 3.7 mg); CAL‐B (230 mg, 70 mm cartridge); solvent (1 mL); 1.1 equiv acetic anhydride (1.2 μL); 60 °C; 0.1 mL min−1 flow rate; 1 bar; 1 cycle. [b] According to HPLC.