HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → 6-Chloro-2-methyl-1H-indole-3-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 59657516 | HCID 59657516 | — |
| Solvent | Water | HCID 962 | — |
| Product | 6-Chloro-2-methyl-1H-indole-3-carboxylic acid | HCID 45121065 | 31% |
Reaction Steps
A solution of 0.57 g (2.2 mmol) 1-(6-chloro-2-methyl-1H-indol-3-yl)-2,2,2-trifluoro-ethanone in 21.7 ml (86.8 mmol) aqueous 4 M sodium hydroxide solution was heated at reflux for 45 min. After cooling to room temperature the reaction mixture was diluted with water and extracted with tert-butyl methyl ether (2×50 ml). The aqueous layer was cooled to 0-5° C., acidified (pH 1-2) with concentrated aqueous hydrochloric acid solution and extracted with ethyl acetate (3×100 ml). The combined ethyl acetate layers were dried over sodium sulfate and concentrated in vacuo to give the title compound (0.14 g, 31%) as an off-white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07332501B2 |
| Source dataset | uspto-grants-2008_02 |
| ORD ID | ord-a821773bf34044d4b42d13f3a9b09f76 |
| Source note | uspto-grants-2008_02 |