TABLE 1.
Entry | Alcohol | Solvent | Temp. (°C) | Time (days) | Alcohol (eq.) | CTMS (eq.) | Yield (%) a |
---|---|---|---|---|---|---|---|
1 | 1 | DCM | r.t. | 2 | 10 | 2.5 | 30 |
2 | 1 | THF | r.t. | 6 | 10 | 2.5 | 42 |
3 | 1 | THF | 40°C | 6 | 10 | 2.5 | 65 |
4 | 1 | THF | 40°C | 6 | 5 | 3.5 | 40 |
5 | 1 | THF | Reflux | 2 | 3.4 | 7.8 | 27 |
6 | 1 | THF | Reflux | 3 | 3.4 | 7.8 | 36 |
7 | 2 | THF | 40°C | 6 | 10 | 2.5 | 15 |
8 | 3 | THF | 40°C | 6 | 10 | 2.5 | 50 |
9 | 4 | THF | 40°C | 6 | 10 | 2.5 | 55 |
Isolated yields.