HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 23114553, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 23114596 | HCID 23114596 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 23114553 | HCID 23114553 | 18% |
Reaction Steps
To an ethanol (10 ml) solution of the 2,5-dichloro-4-[(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl]pyridine (524 mg, 1.17 mmol) obtained in Example 57 was added hydrazine monohydrate (2 ml). The resulting mixture was heated under reflux for 3 hours. After cooling to room temperature, the reaction mixture was concentrated under reduced pressure. The residue thus obtained was subjected to silica gel column chromatography. The fraction obtained from the hexane:ethyl acetate (=1:1) eluate was concentrated under reduced pressure to afford a pale yellow oil. To the resulting oil was added hexane-ether and the solid thus precipitated was collected by filtration to give the title compound (95 mg, 0.214 mmol, 18%) as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07932271B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-daf013c410184d72bf647b64499a4f06 |
| Source note | uspto-grants-2011_04 |