HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → HCID 178490032, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| Reactant | 2-(2-Chloropyridin-5-yl)-1-(3-methoxy-5-methylphenyl)ethanone | HCID 50898941 | — |
| Product | HCID 178490032 | HCID 178490032 | 62% |
Reaction Steps
The keto-enol compound (7.28 g, 26.5 mmol) prepared in Example 63 was refluxed for 12 hours with N,N-dimethylformamide dimethylacetal (24 mL, 204 mmol). Excess N,N-dimethylformamide dimethylacetal was removed by vacuum distillation, and the reaction mixture was dissolved in anhydrous ethanol (150 mL). To this solution was dropwise added hydrazine hydrate (2.65 g, 53 mmol), and stirred at room temperature for 4 hours. The solvent was removed by vacuum distillation. The concentrate was purified through column chromatography (silica gel, ethyl acetate-hexane, 1:2, v/v) to afford the title compound as a red liquid (4.92 g, 62%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08273880B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-d0c025a750ea4ae8a3246436b50a287a |
| Source note | uspto-grants-2012_09 |