Table 1.
The optimisation of conditions for the preparation of compound 9–8.
| ||||
|---|---|---|---|---|
| Entry | Heating | Temp (∘C) | Time (min) | Yield (%) |
| 1a | Oil bath | Reflux | 60 | Trace |
| 2a | Oil bath | Reflux | 360 | 10c |
| 3a | Oil bath | Reflux | 600 | 30c |
| 4a | Oil bath | Reflux | 720 | 41c |
| 5a | Oil bath | Reflux | 960 | 52d |
| 6b | MW | 120 | 20 | 45c |
| 7b | MW | 130 | 10 | 50d |
| 8 b | MW | 130 | 20 | 67 d |
| 9b | MW | 130 | 30 | 62d |
| 10b | MW | 140 | 20 | 60d |
Reaction conditions: ethyl 2-((3-bromophenyl)amino)-2-oxoacetate (1 mmol), Ph3P (1.5 mmol), CCl4 (5 ml).
Reaction conditions: ethyl 2-((3-bromophenyl)amino)-2-oxoacetate (1 mmol), Ph3P (1.5 mmol), CCl4 (5 ml), MW.
The yields were determined by HPLC.
Isolated yields.