HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Bromine → 4-bromo-9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Bromine | HCID 24408 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one | HCID 21990923 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 4-bromo-9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one | HCID 21990872 | — |
Reaktionsschritte
A solution of 9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one (555 mg, 1.82 mmol) in anhydrous dichloromethane (18.2 mL) was treated with sodium bicarbonate (765 mg, 9.1 mmol) and bromine (0.093 mL, 1.82 mmol). The mixture was stirred at room temperature for 30 minutes and then diluted with CH2Cl2 (50 mL) and washed with water (50 mL). The organic phase was dried over MgSO4, filtered through a pad of silica gel (10 mL) with a 10 mL CH2Cl2 rinse, and the solvent evaporated under vacuum. The residue (0.55 g) was lyophilized from benzene to afford 4-bromo-9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one as an amorphous solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07087599B2 |
| Quelldatensatz | uspto-grants-2006_08 |
| ORD ID | ord-9cf6287b0a4c41f28bee99b9776571b1 |
| Quellennotiz | uspto-grants-2006_08 |