HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 4-Bromo-7-methoxy-6-nitro-2,3-dihydro-1H-inden-1-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 4-Bromo-7-hydroxy-6-nitro-2,3-dihydro-1H-inden-1-one | HCID 57781233 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-Bromo-7-methoxy-6-nitro-2,3-dihydro-1H-inden-1-one | HCID 57781263 | 79% |
Reaction Steps
4-Bromo-7-hydroxy-6-nitroindan-1-one (8.07 g, 29.7 mmol) and 1,8-diazabicyclo[5.4.0]undec-7-ene (5.33 mL, 35.6 mmol) were dissolved in N,N-dimethylformamide (150 mL), iodomethane (18.5 mL, 297 mmol) was added, and the mixture was stirred at room temperature for 40 hr. To the reaction solution was added saturated aqueous sodium hydrogencarbonate solution. The mixture was extracted with diethyl ether, washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane=30/70→60/40) to give the title compound (6.70 g, yield 79%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08236837B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-7f1cce1b054e4ba39290809753e88057 |
| Source note | uspto-grants-2012_08 |