The results clearly demonstrate the better reactivity and selectivity of NBS/p-TsOH/CH3CN as a brominating mixture under microwave conditions.
During microwave irradiation of KOH and KOH/phenolic resin mixtures, the sample temperatures increased rapidly, which proved that activated carbon was prepared from the mixture under microwave irradiation.
The results clearly demonstrate the better reactivity and selectivity of NBS/p-TsOH/CH3CN as a brominating mixture under microwave conditions, in fact dibromination or aromatic ring bromination were not observed.
Copper (I) iodide (0.007 mmol, 1.3 mg) and tetrakis triphenylphosphine) palladium(0) (0.0042 mmol, 5 mg) were added to a solution of aryl iodide 47 (0.07 mmol, 42 mg) and alkyne 1 (0.0812 mmol, 11 mg) in degassed DMF (332 μL), iPr2NH (140 μL) and water (28 μL) and the resultant mixture heated under microwave irradiation at 100 °C for 10 min.
Copper (I) iodide (0.25 mmol, 48 mg) and tetrakis triphenylphosphine) palladium(0) (0.15 mmol, 173 mg) were added to a solution of aryl iodide 41 (2.9 mmol, 1.25 g) and alkyne 1 (2.5 mmol, 335 mg) in degassed DMAc (2.5 mL), iPr2NH (500 μL) and water (100 μL) and the resultant mixture heated under microwave irradiation at 100 °C for 10 min.
Copper (I) iodide (0.1 mmol, 19 mg) and tetrakis triphenylphosphine palladium(0) (0.06 mmol, 69 mg) were added to a solution of 4-iodophenylacetic acid (31) (1.16 mmol, 304 mg) and alkyne 1 (1 mmol, 134 mg) in degassed dimethylacetamide (DMAc) (1 mL), iPr2NH (200 μL) and water (40 μL) and the resultant mixture heated under microwave irradiation at 100 °C for 10 min.
Copper (I) iodide (0.1 mmol, 19 mg) and tetrakis triphenylphosphine) palladium(0) (0.06 mmol, 69 mg) were added to a solution of aryl iodide 40 (1.16 mmol, 517 mg) and alkyne 1 (1.0 mmol, 134 mg) in degassed DMAc (1.0 mL), iPr2NH (200 μL) and water (40 μL) and the resultant mixture heated under microwave irradiation at 100 °C for 10 min.
The mixture was heated under microwave irradiating conditions at 110 °C and 300 Watt for 10 min.
After 1 h under argon bubbling, Pd dppf Cl2 CH2Cl2 (0.033 mmol) was introduced and the mixture was stirred under microwave irradiation (monitoring by TLC or by GC MS).
The reaction mixture was stirred under microwave radiation for 1 10 min (hold time) at 50 or 120°C, resulting in the formation of a yellow solid.
Piperidine (0.1 mL) was added dropwise to a mixture of salicylaldehyde (2.0 mL, 18 mmol) and ethyl acetoacetate (3.0 mL, 24 mmol) in EtOH (1.0 mL) The reaction mixture was stirred under microwave irradiation for 5 min (hold time) at 50°C (initial power 20 W) and then was cooled in a stream of compressed air, resulting in a yellow solid.
