HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → 1H-Indole-2-carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Indole-2-carboxylic acid | HCID 72899 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 1H-Indole-2-carboxamide | HCID 594832 | 236.8% |
Reaction Steps
To intermediate 34 G (102.9 mg, 0.24 mmol) in DCM (5 mL) was added 2-indole carboxylic acid (47 mg, 0.29 mmol), HOBT (39 mg, 0.29 mmol), EDC (56 mg, 0.29 mmol) and 2d triethylamine. The reaction mixture was stirred for 16 h, diluted with EtOAc (100 mL), washed with saturated NaHCO3 (2×20 mL), 1N aqueous HCl (2×20 mL), brine (1×20 mL), dried (MgSO4), and concentrated to give the indole amide (110 mg, 80%). Rf =0.58 (10% methanol/DCM); 1HNMR (300 MHz, CDCl3) d 1.04 (d, J=6.8 Hz, 3H), 1.06 (d, J=6.8 Hz, 3H), 1,39 (s, 6H), 3.58 (d, J=16.6 Hz, 1H), 3.83 (s, 3H), 4.59 (d, J=16.6 Hz, 1H), 4.76 (d, J=8.5 Hz, 1H), 5.03 (m, 1H), 6.89 (m, 2H), 6.98 (m, 3H), 7.13 (m, 2H), 7.45 (m, 3H), 7.61 (m, 2H), 8.98 (s, 1H); MS(FAB) m/z 571.2 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06096885 |
| Source dataset | uspto-grants-2000_08 |
| ORD ID | ord-b4c943745d624eb9a1292170d3282569 |
| Source note | uspto-grants-2000_08 |