HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → HCID 54395130, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Epichlorohydrin | HCID 7835 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 2-Hydroxy-1-(4-(hydroxyethoxy)phenyl)-2-methyl-1-propanone | HCID 86266 | — |
| Katalysator | Tetrabutylammonium hydrogen sulfate | HCID 94433 | — |
| Lösungsmittel | 1,2-Dimethoxyethane | HCID 8071 | — |
| Produkt | HCID 54395130 | HCID 54395130 | — |
Reaktionsschritte
Epichlorohydrin (24 g, 0.261 mol) is added to a mixture of 16.31 g (0.408 mol) of sodium hydroxide, 45 ml of water, and 0.761 g (2.24 mmol) of tetrabutylammonium hydrogen sulfate that is previously cooled in an ice-water bath for 20 minutes. To this mixture is added dropwise over 45 minutes with rapid stirring, a solution of 10.32 g (46.0 mmol) of 2-hydroxy-1-[4-(2-hydroxy-ethoxy)phenyl]-2-methylpropan-1-one in 95 ml of 1,2-dimethoxyethane. The reaction mixture is stirred overnight at room temperature. The aqueous layer is removed, and the organic layer is concentrated. Purification by flash chromatography on silica gel (1:1 heptane:ethyl acetate) affords 9.20 g (71% of theoretical yield) of the title compound, a pale yellow liquid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08367743B2 |
| Quelldatensatz | uspto-grants-2013_02 |
| ORD ID | ord-7c56b95367ff400fbe725bfb25a67097 |
| Quellennotiz | uspto-grants-2013_02 |