HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 19436801, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 19436792 | HCID 19436792 | — |
| Reactant | Tri(butyl)vinyltin | HCID 53438229 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19436801 | HCID 19436801 | 91% |
Reaction Steps
5-Bromo-3-[[1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl]oxy]pyridazine (2.0 g, 0.0066 mole), tributylvinyltin (2.3 g, 0.00726 mole) and Pd(PhCH2)Cl(Ph3P)2 (0.1 g, 0.000132 mole) were heated at 100° C. in DMF (75 mL) for 1 hour. The mixture was then poured into ethyl acetate and extracted 2×200 mL with aqueous KF, brine, dried (MgSO4), filtered through a pad of silica gel with ethyl acetate and evaporated in vacuo. The crude oil was purified by silica gel chromatography to give 5-ethenyl-3-[[1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl]oxy]pyridazine (1.62 g, 91% yield) as an off-white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05536701 |
| Source dataset | uspto-grants-1996_07 |
| ORD ID | ord-3dd0bd3c5bc1456ab4980e8c4ce5560f |
| Source note | uspto-grants-1996_07 |