HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 67400720, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 67402350 | HCID 67402350 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 67400720 | HCID 67400720 | 41% |
Reaction Steps
6-Methoxy-3-nitro-2-[2,2,2-trifluoro-1-(pyridin-3-yl)-ethoxy]pyridine (243 mg, 0.738 mmol) was dissolved in acetic acid (3.6 mL) and water (3.6 mL). To this, reduced iron (124 mg, 2.21 mmol) was added under a nitrogen atmosphere at room temperature and the mixture was stirred for 1.7 hours. After water and brine were added to the reaction mixture, extraction with ethyl acetate was performed, followed by washing with saturated sodium bicarbonate and brine, and drying over anhydrous sodium sulfate. The solvent was evaporated off under reduced pressure, and the residue was purified by preparative thin-layer chromatography (chloroform/methanol=30/1) to give Compound HA (89.6 mg, yield: 41%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08673908B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-79981f83432641369e9fa2d02a8a5132 |
| Source note | uspto-grants-2014_03 |