HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrogen Peroxide → 2-(3,5-Dichloro-1-oxido-pyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),3'-oxetane]-6-yl}ethanone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrogen Peroxide | HCID 784 | — |
| Edukt | 2-(3,5-Dichloropyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),3'-oxetane]-6-yl}ethanone | HCID 25005168 | — |
| Katalysator | Manganese dioxide | HCID 14801 | — |
| Katalysator | HCID 178477782 | HCID 178477782 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2-(3,5-Dichloro-1-oxido-pyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),3'-oxetane]-6-yl}ethanone | HCID 25005169 | — |
Reaktionsschritte
To a solution of 2-(3,5-Dichloropyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),3′-oxetane]-6-yl}ethanone [121] (20.5 mg, 50 μmol) in CH2Cl2 (1 mL) was added 30% H2O2 (15 μL) and methyltrioxorhenium(VII) (5 mg). The mixture was stirred for 18 h, added MnO2 (5 mg) and was stirred for another hour. CH2Cl2 (10 mL) was added and the organic phase was washed with water. The combined organic phase was dried over MgSO4 and evaporated to dryness under reduced pressure. Standard HPLC purification afforded 14 mg of the product.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08338431B2 |
| Quelldatensatz | uspto-grants-2012_12 |
| ORD ID | ord-0eb6c5e22bcb453e93177ccfb4df0523 |
| Quellennotiz | uspto-grants-2012_12 |