HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dichloromethane → Tadalafil Impurity 11
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | Piperonal | HCID 8438 | — |
| Edukt | methyl (2R)-2-amino-3-(1H-indol-3-yl)propanoate hydrochloride | HCID 11448200 | — |
| Lösungsmittel | Sulfolane | HCID 31347 | — |
| Produkt | Tadalafil Impurity 11 | HCID 44250481 | — |
Reaktionsschritte
D-tryptophan methyl ester hydrochloride of Step 1 (100 g) and piperonal (65 g) were suspended in sulfolane (500 mL) at 25° C. to 30° C. The reaction mixture was heated to 80° C. to 85° C., stirred for 14 hours, and then cooled to 25° C. to 30° C. To the cooled mixture, dichloromethane (500 mL) was added and the resultant mixture was stirred continuously for 1 hour. The solid obtained was filtered, washed with dichloromethane (500 mL), and dried in air at 40° C. to 45° C. to afford cis 1-benzo[1,3]dioxol-5-yl-2,3,4,9-tetrahydro-1H-beta-carboline-3-carboxylic acid methyl ester hydrochloride.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08871932B2 |
| Quelldatensatz | uspto-grants-2014_10 |
| ORD ID | ord-8b682bd17854417093b72289a6c1f573 |
| Quellennotiz | uspto-grants-2014_10 |