HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
beta-Alanine, ethyl ester, hydrochloride → 10-(2-Ethoxycarbonylethylamino)-7-chloro-2,3-dihydropyridazino[4,5-b]quinoline-1,4-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | beta-Alanine, ethyl ester, hydrochloride | HCID 458475 | — |
| Edukt | 7-Chloro-2,3-dihydro-10-hydrazinopyridazino[4,5-b]quinoline-1,4-dione hydrochloride | HCID 18929905 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Pyridine | HCID 1049 | — |
| Produkt | 10-(2-Ethoxycarbonylethylamino)-7-chloro-2,3-dihydropyridazino[4,5-b]quinoline-1,4-dione | HCID 18929941 | 13% |
Reaktionsschritte
A mixture of 7-chloro-2,3-dihydro-10-hydrazinopyridazino[4,5-b]quinoline-1,4-dione hydrochloride (1.0 g, 2.9 mM, as prepared in Example 44) and beta alanine ethyl ester hydrochloride (49.0 g, 320 mM) in pyridine (52 mL) was refluxed for 23 hr. After cooling, the vigorously stirred reaction mixture was diluted slowly with water (100mL) and then filtered to separate a fine red solid. The collected solids were washed with water and chromatographed (eluant: methanol/methylene chloride; 5/95) over silica gel to provide the title ester (0.13 g, 13%) as a red powder, mp 258°-260° C.; MS(CI): 363 (M+H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05733910 |
| Quelldatensatz | uspto-grants-1998_03 |
| ORD ID | ord-3dd4f599f9304ea3aa6b0fcf1031451d |
| Quellennotiz | uspto-grants-1998_03 |