HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Nitrate → 5,5-dimethyl-8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Nitrate | HCID 24434 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 5,5-dimethyl-2,3,4,5-tetrahydro-1H-1-benzazepine | HCID 57470255 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | 5,5-dimethyl-8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine | HCID 57470256 | 86.8% |
Reaction Steps
At 0° C., KNO3 (0.76 g, 7.54 mmol) was added portionwise to a solution of 5,5-dimethyl-2,3,4,5-tetrahydro-1H-benzo[b]azepine (1.1 g, 6.28 mmol) in H2SO4 (15 mL). After stirring 15 min at this temperature, the mixture was poured into ice water, basified with sat. NaHCO3 to pH 8 and extracted with EtOAc. The organic layer was washed with brine, dried over Na2SO4 and concentrated to give crude 5,5-dimethyl-8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine (1.2 g), which was used directly in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08324242B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-31fdedc658e64654bbb06057dc76cabb |
| Source note | uspto-grants-2012_12 |