HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → N-(2,6-dichloro-4-cyanophenyl)acetamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Acetyl chloride | HCID 6367 | — |
| Edukt | 4-Amino-3,5-dichlorobenzonitrile | HCID 522706 | — |
| Edukt | Sodium bis(trimethylsilyl)amide | HCID 2724254 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | N-(2,6-dichloro-4-cyanophenyl)acetamide | HCID 2735977 | — |
Reaktionsschritte
Step AT1. To a solution of 3,5-dichloro-4-amino-benzonitrile (187 mg, 1 mmol) in 4 mL of THF at room temperature was added 2.2 mL of 1.0 M NaHMDS in THF. The resulting reaction mixture was stirred at room temperature for 30 min., at which time acetyl chloride (3.1 mmol) was added. DCM (100 mL) and water (100 mL) were added to the reaction mixture after being stirred overnight, followed by the addition of 5 mL of 1.4 N HCl aqueous solution. Layers were separated and the aqueous layer was extracted with DCM (2×100 mL). The extracts were combined and solvents were evaporated in vacuo. The residue was purified by HPLC to give 4-acetamido-3,5-dichloro-benzonitrile.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07612069B2 |
| Quelldatensatz | uspto-grants-2009_11 |
| ORD ID | ord-46d39d059dab474da8c8e5ddd82a93c6 |
| Quellennotiz | uspto-grants-2009_11 |