HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylamine → N-ethyl-2-chloro-5-nitrobenzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylamine | HCID 6341 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Chloro-5-nitrobenzoic acid | HCID 17287 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | N-ethyl-2-chloro-5-nitrobenzamide | HCID 4380195 | 45.5% |
Reaction Steps
2-Chloro-5-nitrobenzoic acid (20 g, 100 mmol) in THF (200 mL) was treated with carbonyldiimidazole (CDI) (17.8 g, 110 mmol) and triethylamine (16 mL, 110 mmol) at room temperature. After 1 hr, a solution of ethylamine (70% in water, 10 mL) was added and the mixture was stirred for 18 h. Solvent was removed by evaporation and the residue was dissolved in methylene chloride, washed with 3% KOH solution followed by water (three times) until the aqueous phase extracts were colorless. The organic phase was dried over MgSO4, filtered, and the filtrate was concentrated to provide 10.4 g of N-ethyl-2-chloro-5-nitrobenzamide as light yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06200995B1 |
| Source dataset | uspto-grants-2001_03 |
| ORD ID | ord-3ddae9d5228c41d180ff2e018c39c1f3 |
| Source note | uspto-grants-2001_03 |