HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Pyridine → 5-[Acetyl-(3,5-bis-trifluoromethyl-benzyl)-amino]-8-chloro-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid tert-butyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Pyridine | HCID 1049 | — |
| Edukt | Acetyl chloride | HCID 6367 | — |
| Edukt | 5-(3,5-Bis-trifluoromethyl-benzylamino)-8-chloro-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid tert-butyl ester | HCID 86616082 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 5-[Acetyl-(3,5-bis-trifluoromethyl-benzyl)-amino]-8-chloro-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid tert-butyl ester | HCID 59003107 | 71% |
Reaktionsschritte
Add acetyl chloride (0.3 mmol) followed by pyridine (0.3 mmol) to a solution of 5-(3,5-Bis-trifluoromethyl-benzylamino)-8-chloro-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid tert-butyl ester (0.05 g, 0.1 mmol) in dichloromethane (1 mL). After stirring at room temperature for 24 h remove solvent under vacuum. Chromatograph the product over silica gel using ethyl acetate/hexane (10-40%) to elute. This affords the title compound (0.04 g, 71%) as an oil which foams under vacuum: MS (ES+): 563 (M−H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07749992B2 |
| Quelldatensatz | uspto-grants-2010_07 |
| ORD ID | ord-5b297eeb3da74fba8a7fb3a7e63c2da1 |
| Quellennotiz | uspto-grants-2010_07 |