HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Acetate → 1-(3,3-Dimethyl-6-nitroindolin-1-yl)ethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | Sodium Formate | HCID 2723810 | — |
| Reactant | N-(2-bromo-5-nitrophenyl)-N-(2-methylprop-2-en-1-yl)acetamide | HCID 21959573 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Catalyst | Tetraethylammonium chloride monohydrate | HCID 16211205 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 1-(3,3-Dimethyl-6-nitroindolin-1-yl)ethanone | HCID 16127418 | 88% |
Reaction Steps
A solution of N-(2-bromo-5-nitrophenyl)-N-(2-methylprop-2-enyl)acetamide (3.1 g, 10.2 mmol), tetraethylammonium chloride hydrate (2.4 g, 149 mmol), sodium formate (1.08 g, 18 mmol), sodium acetate (2.76 g, 34.2 mmol) and palladium acetate (0.32 g, 13.2 mmol) in anhydrous DMF (50 mL) was stirred at 80° C. for 15 h under N2 atmosphere. After cooling, the mixture was filtered through Celite. The Celite was washed with EtOAc and the combined filtrates were washed with sat. NaHCO3. The separated organic layer was washed with water and brine, dried over MgSO4, filtered and concentrated under reduced pressure to provide 1-(3,3-dimethyl-6-nitroindolin-1-yl)ethanone as a brown solid (2.1 g, 88%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08741925B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-98644ab522d74a2089080845fe34b7ff |
| Source note | uspto-grants-2014_06 |