HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 154041398, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 9879787 | HCID 9879787 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 154041398 | HCID 154041398 | 70.1% |
Reaction Steps
(E)-1-(4-methanesulfonyl-benzylidene)-3,4-dihydro-1H-naphthalene-2-one (50 mg, 0.16 mmol) and hydroxylamine hydrochloride salt (22 mg, 0.32 mmol) was added into pyridine (2.0 ml) and then stirred overnight at reflux condition. Cooled to room temperature, dichloromethane (40 ml) was added, washed twice using 2 N hydrochloric acid (40 ml) and again washed twice using the saturated brine, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was made to solid by adding diisopropylether and n-hexane, filtrated and dried. As a result, 36.7 mg of the present compound (productive yield 70%) was obtained as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06768019B2 |
| Source dataset | uspto-grants-2004_07 |
| ORD ID | ord-5c71bb88438c4d1db4b8e2ffc50017fe |
| Source note | uspto-grants-2004_07 |