Table 1.
| ||||
---|---|---|---|---|
entry | boronic acid | KF | added water | yield (%)a |
1 | recrystallized from water | dryb | none | 96 |
2 | driedc | dryb | none | 14 |
3 | driedc | dryb | 1 equiv | 87 |
4 | driedc | dryb | 2 equiv | 88 |
5 | driedc | dryb | 4 equiv | 92 |
6 | driedc | dihydrate | none | 94 |
7 | recrystallized from water | dihydrate | none | 97 |
8 | as received | dihydrate | none | 97 |
9 | recrystallized from water | dihydrate | 2 equiv | 97 |
All data are the average of two experiments.
The yield was determined by 1H NMR spectroscopy vs. an internal standard.
Anhydrous (Aldrich).
Heated at 120 °C at 300 mtorr for 1.0 h.