Screening of reaction conditions, regarding oxidant, oxidant amount, ligand, and ligand amounta.
Entry | Oxidant | Oxidant amount (equiv.) | Ligand | Ligand amount (equiv.) | Yieldb (%) |
---|---|---|---|---|---|
1 | K2S2O8 | 2 | Pyridine | 1.5 | 2 |
2 | Oxygen | 2 | Pyridine | 1.5 | 3 |
3 | H2O2 | 2 | Pyridine | 1.5 | 3 |
4 | CHP | 2 | Pyridine | 1.5 | 3 |
5 | TBHP/decane | 2 | Pyridine | 1.5 | 3 |
6 | TBHP/water | 2 | Pyridine | 1.5 | 3 |
7 | DTBP | 2 | Pyridine | 1.5 | 3 |
8 | TEMPO | 2 | Pyridine | 1.5 | 91 |
9 | TEMPO | 0 | Pyridine | 1.5 | 0 |
10 | TEMPO | 1 | Pyridine | 1.5 | 60 |
11 | TEMPO | 1.5 | Pyridine | 1.5 | 62 |
12 | TEMPO | 2 | Pyridine | 1.5 | 91 |
13 | TEMPO | 2.5 | Pyridine | 1.5 | 93 |
14 | TEMPO | 3 | Pyridine | 1.5 | 93 |
15 | TEMPO | 2 | PDCA | 1.5 | 0 |
16 | TEMPO | 2 | HMTA | 1.5 | 0 |
17 | TEMPO | 2 | Ph3P | 1.5 | 0 |
18 | TEMPO | 2 | 4,4′-Dipyridine | 1.5 | 46 |
19 | TEMPO | 2 | 2-Aminopyridine | 1.5 | 47 |
20 | TEMPO | 2 | PHEN | 1.5 | 56 |
21 | TEMPO | 2 | Triethylamine | 1.5 | 63 |
22 | TEMPO | 2 | TMEDA | 1.5 | 72 |
23 | TEMPO | 2 | Pyridine | 1.5 | 91 |
24 | TEMPO | 2 | Pyridine | 0 | 32 |
25 | TEMPO | 2 | Pyridine | 1 | 62 |
26 | TEMPO | 2 | Pyridine | 1.5 | 91 |
27 | TEMPO | 2 | Pyridine | 2 | 91 |
28 | TEMPO | 2 | Pyridine | 2.5 | 91 |
Reaction conditions: 2-aminobenzylalcohol (0.2 mmol); propiophenone (0.4 mmol); Cu2(OBA)2(BPY) (10 mol%); DMF (0.5 mL); 16 h; CHP: cumyl hydroperoxide; TBHP/decane: tert-butyl hydroperoxide in decane; TBHP/water: tert-butyl hydroperoxide in water; DTBP: di-tert-butylperoxide; PDCA: 2,5-pyridinedicarboxylic acid; HMTA: hexanmethylene tetraamine; PHEN: 1,10-phenanthroline; TMEDA: tetramethylethylenediamine.
GC yield.