HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → Ethyl 6-chloroindole-2-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Ethyl 3-(4-chloro-2-nitrophenyl)-2-oxopropanoate | HCID 11173303 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Ethyl 6-chloroindole-2-carboxylate | HCID 7015027 | — |
Reaction Steps
To crude 3-(4-chloro-2-nitro-phenyl)-2-oxo-propionic acid ethyl ester (151 mmol) in ethanol:glacial HOAc (1:1, v/v, 560 mL) at rt was added iron powder (74.4 g) and the reaction mixture was stirred at reflux for 4 h. The mixture was filtered and evaporated to give a residue which was redistributed in dichloromethane/1N HCl. The organic layer was washed with 1N HCl, NaHCO3, and brine and dried. Evaporation followed by crystallization (DCM) gave 6-Chloro-1H-indole-2-carboxylic acid ethyl ester as a pale yellow solid (16.8 g, 50% over 2 steps).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07906548B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-6b67dc4938034cd990f3c829fc8d756e |
| Source note | uspto-grants-2011_03 |