Table 1.
Entry | Brønsted acid | Solvent | Temp (oC) | Time (h) | Producta |
1 | 1% TFA | DCM | rt | 24 | 0 |
2 | 1% triflic acid | DMF | rt | 24 | 0 |
3 | p-TsOH | Toluene | 120 | 24 | 0 |
4 | AcOH | Ethanol | 100 | 24 | 0 |
5 | 2% MSA | ACN | 80 | 24 | 0 |
6 | 2% MSA | DMF | 120 | 16 | 0 |
7 | 2% triflic acid | ACN | 80 | 24 | 27 |
8 | 2% triflic acid | DMF | 120 | 16 | 87 |
9 | 5% triflic acid | DMF | 120 | 16 | 80 |
10 | 1% triflic acid | DMF | 120 | 16 | 75 |
11 | 0.5% triflic acid | DMF | 120 | 16 | 35 |
abased on HPLC.