HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitric Acid → HCID 68519824, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | HCID 68439065 | HCID 68439065 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 68519824 | HCID 68519824 | — |
Reaction Steps
3-Bromo-2-(3-cyano5-fluorobenzenesulfonyl)-thieno[2,3-b]pyridin-N-oxide (prepared as described in WO 2007/072095) (7.97 g, 19.3 mmol) was boiled at 120° C. with 66% nitric acid (1.22 ml) in acetic acid (25 ml) for 4 hours. The reaction mixture was evaporated and the residue was purified by chromatography (Kieselgel 60, chloroform:methanol=5:0.1). First the starting material was isolated (3.7 g, 47%), than a yellow solid, which was treated with ether (5 ml). After filtration the title compound was isolated (0.72 g, 8.3%). LC-MS: (M+H)+ 459.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08263773B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-70eaff1d157a4bf2b182a854d392d43a |
| Source note | uspto-grants-2012_09 |