HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanesulfonic Acid → 1,4-Bis[5-(3,4,5-trimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanesulfonic Acid | HCID 6395 | — |
| Edukt | 1,4-Bis[5-(3,4,5-trimethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine | HCID 20634924 | — |
| Lösungsmittel | Chloroform ethanol | HCID 21889567 | — |
| Produkt | 1,4-Bis[5-(3,4,5-trimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate | HCID 20634923 | — |
Reaktionsschritte
To a solution of 1,4-bis[5-(3,4,5-trimethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (72.4 g, 0.120 mol) in ethanol-chloroform (1:3, 600 mL) was added methanesulfonic acid (24.9 g, 0.258 mol), and the reaction mixture was concentrated under reduced pressure. The residue was recrystallized from methanol-diethyl ether to yield the title compound as a slightly yellow crystalline powder (melting point: 204.0-206.0° C.) (88.2 g, yield: 92%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06706703B2 |
| Quelldatensatz | uspto-grants-2004_03 |
| ORD ID | ord-780fc6867ddc4e848145f2500a1a1acc |
| Quellennotiz | uspto-grants-2004_03 |