Table 2.
Experiment. | Heating (°C) or MW |
Time, min | Reactant Ratio | Reaction Results | ||
---|---|---|---|---|---|---|
1, mmol | I2, equiv. | DMSO, mL | ||||
1 | 120 | 280 | 0.011 | 18.8 | 1 | mixture of 1 and 7 |
2 | 120 | 240 | 0.007 | 28 | 0.5 | mixture of 1 and 7 |
3 | 120 | 120 | 0.007 | 28 | 1 | decomposition of the mixture |
4 | MW, 50 W | 18 | 0.04 | 5.3 | 1 | mixture of 1 and 7 (50/50) |
5 | MW, 50 W | 28 | 0.04 | 5.3 | 1 | 15 min—7 found, 28 min—decomposition of the mixture |
6 | MW, 45 W | 30 | 0.04 | 5.3 | 1 (autoclave) | mixture of 1 and 7 (minor) |
7 | MW, 45 W | 30 | 0.04 | 5.3 | 2 | no reaction |
8 | MW, 45 W | 30 | 0.01 | 18.8 | 1 | mixture of 1 and 7 (minor) |