HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonia → 1-[5-Chloro-2-(methylsulfonyl)phenyl]methanamine hydrochloride
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | 5-Chloro-2-(methylsulfonyl)benzonitrile | HCID 66970048 | — |
| Katalysator | Cobalt | HCID 104730 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 1-[5-Chloro-2-(methylsulfonyl)phenyl]methanamine hydrochloride | HCID 66969896 | 159,5% |
Reaktionsschritte
(Step 3) To a solution of 5-chloro-2-(methylsulfonyl)benzonitrile obtained in Step 2 (3.8 g) in ethanol (25 ml) was added an 8N solution of ammonia in methanol (5 ml) and Raney cobalt (19 g, wet). The resulting mixture was stirred overnight at room temperature under a hydrogen atmosphere. The reaction mixture was filtered through celite, and the filtrate was concentrated under reduced pressure. To the residue were added ethanol (10 ml) and a 2 M hydrogen chloride-methanol solution (10 ml). The resulting mixture was concentrated under reduced pressure, and the residual solid was collected by filtration and washed with ethyl acetate to give 1-[5-chloro-2-(methylsulfonyl)phenyl]methanamine hydrochloride (3.6 g) as a white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07985863B2 |
| Quelldatensatz | uspto-grants-2011_07 |
| ORD ID | ord-9f6dc038bf034ba5bb52ddd7334f9e19 |
| Quellennotiz | uspto-grants-2011_07 |