HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
N-Methylmorpholine N-oxide monohydrate → 2-Hydroxy-6-methoxy-3,3-dimethyl-2,3-dihydro-1H-benzo[b]pyrano[3,2-h]-acridine-1,7(14H)-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | N-Methylmorpholine N-oxide monohydrate | HCID 2724197 | — |
| Edukt | 6-Methoxy-3,3-dimethyl-3,14-dihydro-7H-benzo[b]pyrano[3,2-h]acridin-7-one | HCID 22064514 | — |
| Edukt | Sodium Bisulfite | HCID 23665763 | — |
| Katalysator | Osmium Tetroxide | HCID 30318 | — |
| Lösungsmittel | tert-Butanol | HCID 6386 | — |
| Lösungsmittel | t-Butanol tetrahydrofuran water | HCID 22124471 | — |
| Produkt | 2-Hydroxy-6-methoxy-3,3-dimethyl-2,3-dihydro-1H-benzo[b]pyrano[3,2-h]-acridine-1,7(14H)-dione | HCID 22064508 | — |
Reaktionsschritte
To a solution of 1.33 mmol of the compound obtained in Step 2 in 30 ml of a 10/3/1 mixture of tert-butanol/tetrahydrofuran/water there are added osmium tetroxide in the form of a 2.5% solution in 0.67 ml of 2-methyl-2-propanol and 1.35 mmol of 4-methylmorpholine-N-oxide monohydrate. After stirring for two days at ambient temperature, NaHSO3 solution is added. After stirring for one hour, the reaction mixture is extracted with dichloromethane. The organic phase is dried, filtered and then evaporated under reduced pressure. Chromatography of the residue over silica gel (dichloromethane/methanol: 98/2) allows the expected product to be isolated.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06642248B2 |
| Quelldatensatz | uspto-grants-2003_11 |
| ORD ID | ord-e2c95e9457c147e1acc8484d8a83ddb9 |
| Quellennotiz | uspto-grants-2003_11 |