HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1-Methylhomopiperazine → 2-[4-(4-Methylhexahydro-1,4-diazepin-1-yl)piperidin-1-ylcarbonyl]amino-N-(5-chloropyridin-2-yl)benzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1-Methylhomopiperazine | HCID 228349 | — |
| Edukt | Sodium cyanoborohydride | HCID 5003444 | — |
| Edukt | N-(5-Chloropyridin-2-yl)-2-(4-oxopiperidin-1-ylcarbonyl)aminobenzamide | HCID 21906655 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 2-[4-(4-Methylhexahydro-1,4-diazepin-1-yl)piperidin-1-ylcarbonyl]amino-N-(5-chloropyridin-2-yl)benzamide | HCID 21075306 | — |
Reaktionsschritte
A solution of N-(5-chloropyridin-2-yl)-2-(4-oxo-piperidin-1-ylcarbonyl)aminobenzamide (100 mg, 0.268 mmol) and 4-methyl(hexahydro-1,4-diazepine) (0.03 mL, 0.241 mmol) in 10% acetic acid in methanol (2.2 mL) was treated with sodium cyanoborohydride (20 mg, 0.268 mmol). After 15 h, the mixture was loaded onto a SCX column, which was pretreated with a solution of 5% acetic acid in methanol. The column was eluted with methanol followed by 2 N ammonia in methanol. The eluent was concentrated to afford title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07163938B2 |
| Quelldatensatz | uspto-grants-2007_01 |
| ORD ID | ord-f11a75d437d447ea94c534a460c374b2 |
| Quellennotiz | uspto-grants-2007_01 |