Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Epithiochlorohydrin | HCID 18588 | — |
| Edukt | 1,3-dihydroxy-12H-benzo(b)xanthen-12-one | HCID 10707705 | — |
| Lösungsmittel | Acetone | HCID 180 | — |
| Produkt | HCID 46232618 | HCID 46232618 | 20,8% |
Reaktionsschritte
1,3-dihydroxy-12H-benzo[b]xanthen-12-one (0.05 g, 0.18 mmol) synthesized in Step 1 of Example 18, K2CO3 (0.07 g, 0.54 mmol), and anhydrous acetone (18 mL) were charged to a dry round-bottom flask. Under stirring, epithiochlorohydrin (0.07 g, 0.72 mmol) dissolved in anhydrous acetone (2 mL) was added thereto. The reaction liquid was stirred with reflux at a temperature of 55 to 60° C. under a nitrogen atmosphere (overnight). Solid of the reaction mixture was filtered and removed, and the filtrate was concentrated under reduced pressure. The resulting residue was separated and purified by silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=1:3 (v/v)) to give the title compound (13.1 mg, 20.8%) as a yellow solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US08846749B2 |
|---|
| Quelldatensatz | uspto-grants-2014_09 |
|---|
| ORD ID | ord-847200c51ac644d7879d0a32c9faa962 |
|---|
| Quellennotiz | uspto-grants-2014_09 |
|---|