HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxylamine HCl → HCID 86690535, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxylamine HCl | HCID 21645 | — |
| Reactant | HCID 67130098 | HCID 67130098 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 86690535 | HCID 86690535 | 76% |
Reaction Steps
To [11-(2-ethyl-hexyl)-5-nitro-11H-benzo[a]carbazole-8-yl]-o-tolyl-methanone (0.36 g, 0.73 mmol) in pyridine (6 ml) is added hydroxylammonium chloride (0.10 g, 1.45 mmol) at 120° C. After stirring for 16 hours, the reaction mixture is poured into ice-water. The crude is extracted with AcOEt, and washed with water and brine. After drying over MgSO4 and concentration, the crude is purified by column chromatography on silica gel eluting with CH2Cl2 to obtain a yellow resin (0.28 g, 76%). The structure is confirmed by 1H-NMR spectrum (CDCl3). δ [ppm]: 0.79-0.90 (m), 1.13-1.48 (m), 2.21 (m), 2.29 (s), 4.69 (m), 7.25 (d), 7.37-7.47 (m), 7.55 (d), 7.67-7.75 (m), 7.90 (d), 8.04 (s), 8.60 (d), 8.89 (d), 8.92 (s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09051397B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-2a58e31bd88d481887cd50b84d0a654d |
| Source note | uspto-grants-2015_06 |