HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → (+/-)-4-(4-Chlorobenzyl)-2-[(4-chloro-2-methoxyphenoxy)methyl]morpholine oxalic acid salt
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 4-Chloroguaiacol | HCID 28050 | — |
| Edukt | 18-Crown-6 | HCID 28557 | — |
| Edukt | Morpholine, 2-(chloromethyl)-4-[(4-chlorophenyl)methyl]- | HCID 11345975 | — |
| Edukt | Potassium ethoxide | HCID 23670592 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | (+/-)-4-(4-Chlorobenzyl)-2-[(4-chloro-2-methoxyphenoxy)methyl]morpholine oxalic acid salt | HCID 69687298 | — |
Reaktionsschritte
A mixture of (±)-4-(4-chlorobenzyl)-2-chloromethyimorphoiine (10.0 g 38.5 mmol), 4-chloro-2-methoxyphenol (9.0 g, 58 mmol), potassium ethoxide (6.5 g, 77 mmol), and 18-crown-6 (10.2 g, 38.5) was refluxed in toluene (100 ml) for 34 h. Water (200 ml) was added and the phases were separated. Drying and evaporation of the toluene phase was followed by column chromatography on silica gel with 3% ethanol in dichloromethane as eluent. The free base was dissolved in ether and precipitated with oxalic acid to give the title compound. Yield 10.3 g, 57%, mp 133-139° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06479491B1 |
| Quelldatensatz | uspto-grants-2002_11 |
| ORD ID | ord-c4b63b09980c4d7aa532036efc2c466f |
| Quellennotiz | uspto-grants-2002_11 |