1. Optimization of the Conditions for the Reaction of 2a .
| entry | NaBArF 24 (mol%) | solvent | additive | 3a yield (%) |
|---|---|---|---|---|
| 1 | 10 | DCM | 41 | |
| 2 | 10 | DCM | 35 | |
| 3 | 10 | DCM | 41 | |
| 4 | 10 | DCM | 4Å MS | 49 |
| 5 | 10 | DCM | 4Å MS | 29 |
| 6 | 10 | DCM | 4Å MS | 40 |
| 7 | 20 | DCM | 4Å MS | 32 |
| 8 | 5 | DCM | 4Å MS | 28 |
| 9 | 10 | CHCl3 | 4Å MS | 39 |
| 10 | 10 | DCE | 4Å MS | 45 |
| 11 | 10 | THF | 4Å MS | 18 |
| 12 | 10 | MeCN | 4Å MS | 1 |
| 13 | 10 | Acetone | 4Å MS | -- |
| 14 | 10 | DCM | 4Å MS | 33 |
| 15 | 10 | DCM | 4Å MS | 37 |
| 16 | 10 | DCM | 4Å MS | 28 |
Conditions: NaBArF 24 (x mol%), 1b-Cl (1.0 equiv), 2a (0.2 mmol, 1.0 equiv), and 4Å MS (60 mg; 300 mg/mmol) as additive (if used) in the corresponding solvent [0.1 M] were reacted at r.t. (∼23 °C) for 72 h under argon atmosphere.
Isolated yield.
Use of 10 mol% of KBArF 20 as the catalyst.
Use of 1.5 equiv of 1b-Cl.
Addition of 180 mg (900 mg/mmol) of 4Å MS.
24 h reaction.
6 days reaction time.
Reaction at 0 °C.
Reaction at 40 °C.
Reaction at 80 °C.
