HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 58765320, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | HCID 22735319 | HCID 22735319 | — |
| Solvent | Acetic Anhydride | HCID 7918 | — |
| Product | HCID 58765320 | HCID 58765320 | — |
Reaction Steps
A solution of 6-trifluoromethoxy-quinoline 1-oxide of Step B (4.58 g, 20 mmol) in acetic anhydride (20 mL) is heated at 135° C. under nitrogen for 4 hours. The mixture is poured onto ice, carefully basified with sodium carbonate and extracted with ethyl acetate. The extracts are washed with brine, dried over anhydrous magnesium sulfate and evaporated to dryness. The residue is flash chromatographed on silica Merck-60 using a gradient of methanol (0–3%) in hexane-ethyl acetate (1:1). The appropriate fractions are combined and evaporated. The residue is triturated with diethyl ether. The insoluble is collected, washed with hexane and dried to provide the title compound as a pale brown crystalline solid (1.086 g), m.p. 215–217° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07153849B2 |
| Source dataset | uspto-grants-2006_12 |
| ORD ID | ord-f0a4a0c6691648ed8ecd8419c4172393 |
| Source note | uspto-grants-2006_12 |