HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,2-Dichloroethane → 2-Amino-3-bromo-5-methylbenzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,2-Dichloroethane | HCID 11 | — |
| Edukt | Ammonium Chloride | HCID 25517 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | HOAt | HCID 181649 | — |
| Edukt | 2-Amino-3-bromo-5-methylbenzoic acid | HCID 2774400 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 2-Amino-3-bromo-5-methylbenzamide | HCID 58828874 | 89,3% |
Reaktionsschritte
2-amino-3-bromo-5-methylbenzoic acid (2.06 g, 8.95 mmol) was dissolved in DMF (19 ml) and EDC (2.10 g, 11.0 mmol), HOAt (1.56 g, 11.5 mmol), ammonium chloride (2.03 g, 38.0 mmol), and iPr2NEt (6.5 ml, 37.3 mmol) were added. The reaction was stirred at room temperature under nitrogen for 21.5 hours, and then poured into water (50 ml), resulting in the formation of a precipitate. The suspension was filtered and the solid was washed with water and dried in vacuo to give title compound (1.83 g, 89%). MS (ESI pos. ion) m/z: 229 (M+H). Calc'd Exact Mass for C8H9BrN2O: 228.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08017601B2 |
| Quelldatensatz | uspto-grants-2011_09 |
| ORD ID | ord-9093f35b167a4834a7cfc00ac1b92d4d |
| Quellennotiz | uspto-grants-2011_09 |