HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium hydroxide monohydrate → HCID 22708342, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium hydroxide monohydrate | HCID 23719240 | — |
| Edukt | HCID 86615847 | HCID 86615847 | — |
| Lösungsmittel | Isopropanol | HCID 3776 | — |
| Produkt | HCID 22708342 | HCID 22708342 | — |
Reaktionsschritte
A solution of 4-hydroxy-6-chloro-8-trifluoromethoxychroman-4-yl carboxylic acid, methyl ester in iso-propanol (50 mL) was added to KOH/H2O (20%, 60 mL) and the mixture was refluxed overnight. The resultant solution was partially concentrated, and the remainder was acidified with H2SO4 (10%). The very turbid mixture was extracted with ether (3×), and the combined organic phase was dried (Na2SO4) and concentrated. The crude product was purified via prep-HPLC (CH3CN:0.1M ammonium acetate (30:60)). The fractions of interest were partly concentrated and extracted with ether. The combined organic layers were washed with water, dried (Na2SO4), and concentrated, yielding 0.24 g (10% over steps (vi)-(ix)).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06750243B1 |
| Quelldatensatz | uspto-grants-2004_06 |
| ORD ID | ord-c0de8a02ad934412b2796506b0bef1b1 |
| Quellennotiz | uspto-grants-2004_06 |