Table 4.
| |||||||
---|---|---|---|---|---|---|---|
Entry | Ar | X | R | Cat. [mol %] | T [°C] | t [h] | Yield [%] |
1 | 4-Tol | Br | octyl | 0.05 | 90 | 2 | 96 |
2b | Br | octyl | 0.05 | 90 | 2 | 98 | |
3 | I | octyl | 0.05 | 70 | 2 | 96 | |
4 | Ph | Br | octyl | 0.05 | 90 | 4 | 98 |
5 | I | octyl | 0.05 | 70 | 4 | 98 | |
6 | 4-anisyl | Br | octyl | 0.05 | 90 | 3 | 98 |
7 | I | octyl | 0.05 | 70 | 3 | 96 | |
8 | Ph | Br | 2-methylbutyl | 0.05 | 90 | 5 | 90 |
9 | I | 2-methylbutyl | 0.05 | 70 | 6 | 96 | |
10 | 3-anisyl | Br | 2-methylbutyl | 0.05 | 90 | 6 | 96 |
11 | I | 2-methylbutyl | 0.05 | 70 | 6 | 96 | |
12 | Ph | Br | sec-butyl | 0.05 | 90 | 4 | 90 |
13 | I | sec-butyl | 0.05 | 70 | 4 | 93 | |
14 | 4-Tol | Br | cyclohexyl | 0.05 | 90 | 6 | 94 |
15 | I | cyclohexyl | 0.05 | 70 | 6 | 99 | |
16 | Br | tert-butyl | 0.05 | 90 | 5 | 93 | |
17 | 4-trifluoromethylphenyl | Br | tert-butyl | 0.05 | 90 | 3 | 79 |
18 | 1-naphthyl | Br | octyl | 0.05 | 90 | 8 | 96 |
19 | I | octyl | 0.05 | 90 | 12 | 93 | |
20 | 2-anisyl | Br | octyl | 0.05 | 110 | 4 | 99 |
21 | I | octyl | 0.05 | 90 | 12 | 96 | |
22 | 2-Tol | Br | octyl | 0.01 | 110 | 12 | 99 |
23 | I | octyl | 0.05 | 70 | 12 | 98 | |
24 | 2,5-dimethylphenyl | I | tert-butyl | 0.05 | 90 | 12 | 93 |
25 | 2,6-dimethylphenyl | Br | tert-butyl | 0.25 | 110 | 4 | 92 |
26 | I | tert-butyl | 0.1 | 110 | 8 | 94 |
All experiments were conducted with a 1:1 ratio of metal to ligand, 1 mmol of both ArX and thiol, and 1.1 equiv of NaOtBu in DME (1.5 mL) at the appropriate temperature.
Reaction performed without using a drybox.