HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetic Acid → trans-6-Aminomethyl-3,4-dihydro-2,2-dimethyl-4-(2-oxopyrrolidinyl)-2H-1-benzopyran-3-ol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Levcromakalim | HCID 93504 | — |
| Edukt | HCID 178418361 | HCID 178418361 | — |
| Katalysator | Palladium | HCID 23938 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | trans-6-Aminomethyl-3,4-dihydro-2,2-dimethyl-4-(2-oxopyrrolidinyl)-2H-1-benzopyran-3-ol | HCID 67883096 | — |
Reaktionsschritte
trans-6-Cyano-3,4-dihydro-2,2-dimethyl-4-(2-oxopyrrolidinyl)-2H-1-benzopyran-3-ol (5 g, prepared as described in J. Med. Chem. 29, 2194 (1986)), in ethanol (375 ml) and glacial acetic acid (75 ml) containing concentrated HCl (5 ml) was shaken in the presence of 10% Pd/C (1 g) in an atmosphere of hydrogen for 4 h. The catalyst was filtered off and the solution neutralised with 10% aqueous NaOH solution, and the solution evaporated to dryness. Acid-base extraction, and drying of a dichloromethane solution of the residue, furnished, after recrystallisation from ethyl acetate-pentane, 2.03 g of the required aminomethyl compound of example 4 of mp 191°-193° C. as the hemihydrate.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05210234 |
| Quelldatensatz | uspto-grants-1993_05 |
| ORD ID | ord-febefecd2d3442c1b3fa194bb07a2d95 |
| Quellennotiz | uspto-grants-1993_05 |