HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → Methyl 3-[(2-bromo-5-methoxybenzoyl)amino]-4-methylbenzoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Methyl 3-amino-4-methylbenzoate | HCID 337778 | — |
| Edukt | 2-Bromo-5-methoxybenzoyl chloride | HCID 2781656 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | Methyl 3-[(2-bromo-5-methoxybenzoyl)amino]-4-methylbenzoate | HCID 2673200 | 73,7% |
Reaktionsschritte
Methyl 3-amino-4-methylbenzoate (3.18 g), 2-bromo-5-methoxybenzene-1-carbonyl chloride (4.8 g) and triethylamine (5.4 ml) in THF (45 ml) were stirred at room temperature for 2.5 hour and then concentrated. The residue was dissolved in ethyl acetate and washed with 1N HCl, water, brine, dried (magnesium sulfate) and concentrated. The residue was recrystallised from hot ethyl acetate, washed with ether, and air dried to yield methyl 3-[(2-bromo-5-methoxybenzoyl)amino]-4-methylbenzoate as a white solid (5.36 g); NMR Spectrum: (DMSOd6) 2.39 (s, 3H), 3.83 (s, 3H), 3.87 (s, 3H), 7.02 (m, 1H), 7.23 (d, 1H), 7.42 (d, 1H), 7.60 (d, 1H), 7.75 (m, 1H), 8.12 (s, 1H), 10.06 (s, 1H); Mass Spectrum: M+H+ 377.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07786115B2 |
| Quelldatensatz | uspto-grants-2010_08 |
| ORD ID | ord-6ea55001b4594ff7bc0ae99132bbd492 |
| Quellennotiz | uspto-grants-2010_08 |