TLIM-catalyzed synthesis of bis(indolyl)methanes.
Entrya | R1 | R2 | R3 | R4 | Product | Time/h | Yieldb/% |
---|---|---|---|---|---|---|---|
1 | H | H | H | 4-ClC6H5 | 3a | 36 | 93(90d) |
2 | H | H | H | 3-NO2-C6H5 | 3b | 36 | 85 |
3 | H | H | H | 4-NO2-C6H5 | 3c | 36 | 87 |
4 | H | H | H | 2-F-C6H5 | 3d | 36 | 99 |
5 | H | H | H | 4-CN-C6H5 | 3e | 36 | 98 |
6 | H | H | H | C6H6 | 3f | 36 | 98 |
7 | H | H | H | 4-CH3-C6H5 | 3g | 36 | 95 |
8 | H | H | H | 4-OCH3-C6H5 | 3h | 36 | 95 |
9 | H | H | H | 4-OH-3-OCH3-C6H4 | 3i | 36 | 88 |
10 | H | H | H | 2-OH-3-OCH3-C6H4 | 3j | 36 | 88 |
11 | H | H | H | C3H7 | 3k | 72 | 87 |
12 | H | H | H | Hc | 3l | 36 | 75 |
13 | H | H | H | 2-Thienyl | 3m | 72 | 89 |
14 | H | H | H | 2-Pyridyl | 3n | 72 | 72 |
15 | H | H | H | 4-t-C4H9-C6H5 | 3o | 72 | 95 |
16 | H | CH3 | H | 4-Cl-C6H5 | 3p | 36 | 96d |
17 | CH3 | H | H | 4-Cl-C6H5 | 3q | 36 | 98d |
18 | OCH3 | H | H | 4-Cl-C6H5 | 3r | 36 | 88d |
19 | Cl | H | H | 4-Cl-C6H5 | 3s | 36 | 90d |
20 | H | H | CH3 | 4-Cl-C6H5 | 3t | 36 | 93d |
21 | H | H | H | 4-Cl-C6H5 | 3a | 36 | 94e |
22 | H | H | H | 4-Cl-C6H5 | 3a | 36 | 86f |
23 | H | H | H | 4-Cl-C6H5 | 3a | 36 | 81g |
24 | H | H | H | 4-Cl-C6H5 | 3a | 36 | 77h |
25 | H | H | H | 4-Cl-C6H5 | 3a | 36 | 74i |
Reaction conditions: TLIM (10 mg), aldehyde (1 mmol), indole (2 mmol), water (5 mL), 55 °C.
HPLC yield.
Reaction conditions: TLIM (10 mg), formaldehyde aqueous solution (37%, 3 mmol), indole (2 mmol), water (5 mL), 55 °C.
Isolated yield.
Reaction conditions: TLIM (100 mg), 4-chlorobenzaldehyde (10 mmol), 1H-indole (20 mmol), water (50 mL), 55 °C, HPLC yield.
HPLC yield of 3a (run 2).
HPLC yield of 3a (run 3).
HPLC yield of 3a (run 4).
HPLC yield of 3a (run 5).