HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 9-(4-Bromobutyl)-N-(2,2,2-trifluoroethyl)-9H-fluorene-9-carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,2,2-Trifluoroethylamine hydrochloride | HCID 9772 | — |
| Reactant | 9-(4-bromo-butyl)-9H-fluorene-9-carboxylic Acid Chloride | HCID 10522758 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 9-(4-Bromobutyl)-N-(2,2,2-trifluoroethyl)-9H-fluorene-9-carboxamide | HCID 10526437 | — |
Reaction Steps
23 g (0.063 mol) of 9-(4-bromo-butyl)-9H-fluorene-9-carboxylic acid chloride are added dropwise at 0° C. under nitrogen to a solution of 9.35 g (0.069 mol) of 2,2,2-trifluoroethylamine-hydrochloride and 26 ml (0.188 mol) of triethylamine in 550 ml of dichloromethane and stirred for 2 hours at ambient temperature. The reaction mixture is extracted twice with water, 1N hydrochloric acid and sodium hydrogen carbonate solution. The organic phase is dried over sodium sulphate and the solvent is distilled off. Purification is by column chromatography on silica gel (eluant: cyclohexane/ethyl acetate=8:1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06818644B1 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-9a5973b7995646bf98e166be081b4ce5 |
| Source note | uspto-grants-2004_11 |