HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 3,5-bis-(1,1-dimethylethyl)-4-hydroxy-N-[2-(4-nitrophenyl)ethyl]-benzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Dicyclohexylcarbodiimide | HCID 10868 | — |
| Reactant | 3,5-Di-tert-butyl-4-hydroxybenzoic acid | HCID 15007 | — |
| Reactant | 4-Nitrophenetylamine hydrochloride | HCID 69003426 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3,5-bis-(1,1-dimethylethyl)-4-hydroxy-N-[2-(4-nitrophenyl)ethyl]-benzamide | HCID 21918633 | 73% |
Reaction Steps
2.02 g (10 mmoles) of 4-nitrophenetylamine hydrochloride, 2.5 g (10 mmoles) of 3,5-di-tert-butyl-4-hydroxy-benzoic acid, 1.38 ml (10 mmoles) of triethylamine and 2.26 g (11 mmoles) of dicyclohexylcarbodiimide are introduced into a 100 ml flask containing 20 ml of THF. The reaction medium is agitated for 15 hours at ambient temperature, the precipitate which appears is filtered out and rinsed with ethyl acetate. After concentration of the filtrate under reduced pressure, the residue is precipitated from diethyl ether. The solid is recovered by filtration and rinsed with diethyl ether. A white powder is obtained with a yield of 73%. Melting point: 204-206° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06630461B2 |
| Source dataset | uspto-grants-2003_10 |
| ORD ID | ord-56e821c666a74dea9608a847c9be7ccc |
| Source note | uspto-grants-2003_10 |