HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → 6-Acetyl-7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 7-Methoxy-1,1-dimethyl-3,4-dihydronaphthalen-2(1H)-one | HCID 13011007 | — |
| Reactant | Aluminum chloride nitrobenzene | HCID 20212918 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 6-Acetyl-7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one | HCID 66834425 | — |
Reaction Steps
To the dichloromethane (70 ml) solution of 7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound A2, 3 g, 14.7 mmol), acetic anhydride (1.7 ml, 1.2 eq.) and aluminum chloride-nitrobenzene solution (1 M, 44 ml, 3 eq.) was added at 0° C., and stirred for 3 hr. Thereafter, the reaction solution was added with saturated aqueous solution of sodium hydrogen carbonate and extracted twice with dichloromethane. The organic layer was washed with brine and dried over magnesium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the title compound as a crude product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09126931B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-0838e2630d57439eb3ed728e84c44d19 |
| Source note | uspto-grants-2015_09 |