HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Cyclopropanecarbonyl chloride → 2-Amino-5-bromo-3-cyano-6-fluoro-4-methylphenyl acetate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Cyclopropanecarbonyl chloride | HCID 77637 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 2-Amino-5-bromo-4-fluoro-3-hydroxy-6-methylbenzonitrile | HCID 86097514 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 2-Amino-5-bromo-3-cyano-6-fluoro-4-methylphenyl acetate | HCID 86097516 | 97,3% |
Reaktionsschritte
2-Amino-5-bromo-4-fluoro-3-hydroxy-6-methylbenzonitrile (I-75) (7.86 g, 32.08 mmol) and diisopropylethylamine (19.5 ml, 112.2 mmol) were dissolved in ethyl acetate (300 ml), and at 0° C., cyclopropanecarbonyl chloride (4.4 ml, 48.12 mmol) was dropwise added, followed by stirring at room temperature for 16 hours under nitrogen atmosphere. After the reaction, ethyl acetate was added to the reaction liquid, followed by washing with water and saturated brine. The organic layer was concentrated under reduced pressure, the resulting residue was recrystallized with diisopropyl ether/ethyl acetate to obtain the entitled compound (8.96 g, 89%) as a white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07737166B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-26668f8c13a84f17b4fc2b4a1d1a64da |
| Quellennotiz | uspto-grants-2010_06 |