HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetonitrile → acrylic acid 4-{2-hydroxy-3-[2-(9-oxo-9H-thioxanthen-2-yloxy)-acetoxy]-propoxy}-butyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetonitrile | HCID 6342 | — |
| Edukt | 2-(Carboxymethoxy)thioxanthone | HCID 3019853 | — |
| Edukt | 4-Hydroxybutylacrylate glycidylether | HCID 22323150 | — |
| Katalysator | 2,6-Di-tert-butyl-4-methylphenol | HCID 31404 | — |
| Katalysator | Tetrabutylammonium Bromide | HCID 74236 | — |
| Lösungsmittel | Dimethylacetamide | HCID 31374 | — |
| Produkt | acrylic acid 4-{2-hydroxy-3-[2-(9-oxo-9H-thioxanthen-2-yloxy)-acetoxy]-propoxy}-butyl ester | HCID 58325515 | 144,2% |
Reaktionsschritte
A reaction mixture containing (9-oxo-9H-thioxanthen-2-yloxy)acetic acid (4.0 g, 14 mmol), acetonitrile (55 ml), dimethylacetamide (10 mL), tetrabutylammonium bromide (0.5 g, 1.4 mmol) and 2,6-di-tert-butyl-4-methylphenol (0.03 g, 0.114 mmol) was heated to reflux. At this temperature 4-hydroxybutylacrylate glycidylether (2.3 g, 11.4 mmol) was added and the mixture was allowed to stir at reflux temperature for 16 hours. The mixture was cooled to room temperature and the solvent was evaporated under reduced pressure to provide 8.0 g of a yellow oil. The product was purified on a Prochrom LC80 Column using Kromasil Si 60A 10 μm as silica and dichloromethane/ethyl acetate (60/40) as eluent, to afford 1.8 g of a yellow oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08536217B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-0d06cbb7a63845c398af753e17c01870 |
| Quellennotiz | uspto-grants-2013_09 |