1 |
1.5 equiv BF3•Et2O, 0.15 M in 3-pentanol, rt |
31% 46, 54% 47
|
2 |
1.2 equiv BF3•Et2O, 0.15 M in 3-pentanol, −20 °C |
20% 46, 41% 47
|
3 |
1.5 equiv BF3•Et2O, 0.15 M in 3-pentanol, 75 °C |
60% 46, 22% 47
|
4 |
1.5 equiv In(OTf)3, 0.15 M in 3-pentanol, 75 °C |
17% 46, 71% 47
|
5 |
10 mol% Cu(OTf)2, 0.1 M in 3-pentanol, 0-rt-100 °C |
87% 47
|
6 |
1.5 equiv BF3•Et2O, 0.15 M in 3-pentanol, 75 °C |
54% 46, 36% 47, 12% 48
|
7 |
1.5 equiv BF3•Et2O, 0.05 M in 3-pentanol, 70 °C |
54% 46, 34% 47, 12% 48
|
8 |
1.5 equiv BF3•Et2O, 0.05 M in 3-pentanol, 3Å MS, 70 °C |
50% 46, 34% 47, 16% 48
|
9 |
1.5 equiv B(OCHEt2)3, 0.15 M in 3-pentanol, 75 °C |
No reaction |
10 |
Azeotropically dired with toluene, then 1.5 equiv BF3•Et2O, 0.15 M in 3-pentanol, 75 °C |
60% 46, 26% 47, 13% 48
|
11 |
1.5 equiv BF3•Et2O, 1 equiv BSA in rxn, 0.15 M in 3-pentanol, rt |
25% 46, 57% 47, 7% 48, 11% starting material |
12 |
Pre-mixed with BSA, volatile fully removed; then 1.5 equiv BF3•Et2O, 0.15 M in 3-pentanol, 75 °C |
65% 46, 20% 47, 15% 48
|