HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → Ethyl acetate hexane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2,6-Dichloro-3-nitropyridine | HCID 85239 | — |
| Reactant | HCID 178507266 | HCID 178507266 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | Ethyl acetate hexane | HCID 21226206 | 85.4% |
| Product | HCID 178526632 | HCID 178526632 | — |
Reaction Steps
A solution of 5-cyclopropyl-2H-pyrazol-3-ylamine (638 mg, 5.18 mmol) in 6 ml of acetonitrile was added dropwise over 10 minutes to a cooled (0 C) mixture of 2,6-dichloro-3-nitro-pyridine (1.0 g, 5.18 mmol) and potassium carbonate (860 mg, 6.22 mmol) in 20 ml of acetonitrile. After the addition, the reaction was warmed to room temperature and stirred for 18 hours. The reaction was filtered and the filtrate evaporated in vacuo to afford a brown residue which was purified by flash chromatography (SiO2) eluting with ethyl acetate-hexane (1:7) 257 mg (17.7% yield) of the desired product (major regioisomer). HPLC Rt 6.09, mins. MS: m/z 280.0 (M+1) 278.1 (M−1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07262200B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-c1dcd7434f9946a793b8c740c6c883ba |
| Source note | uspto-grants-2007_08 |