Table 1 Optimization of reaction conditions
Entry | Solvent | Temperature (°C) | Time | V-5/V-5-2 (mol/mol) |
|---|---|---|---|---|
1 | DCM | 5 | 30 min | 76.0/24.0 |
2 | DCM | 0 | 30 min | 90.9/9.1 |
3 | DCM | − 5 | 30 min | 95.7/4.3 |
4 | DCM | − 10 | 30 min | 97.6/2.4 |
5 | DCM | − 15 | 1.5 h | 97.1/2.9 |
Entry | Solvent | Temperature (°C) | Time | V-5/V-5-2 (mol/mol) |
|---|---|---|---|---|
1 | DCM | 5 | 30 min | 76.0/24.0 |
2 | DCM | 0 | 30 min | 90.9/9.1 |
3 | DCM | − 5 | 30 min | 95.7/4.3 |
4 | DCM | − 10 | 30 min | 97.6/2.4 |
5 | DCM | − 15 | 1.5 h | 97.1/2.9 |