HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Hydroxide → 5-Nitro-6-(2,4-difluorophenylthio)-1-indanone ethylene ketal
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 2,4-Difluorobenzene-1-thiol | HCID 2737073 | — |
| Reactant | HCID 10357417 | HCID 10357417 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | 5-Nitro-6-(2,4-difluorophenylthio)-1-indanone ethylene ketal | HCID 10316757 | 81% |
Reaction Steps
To a mixture of 5-nitro-6-bromo-1-indanone ethylene ketal (600 mg, 2.0 mmol) and 2,4-difluorothiophenol (F. Klages and K. Bott Chem. Ber. 97,735 (1964)) (440 mg, 3.0 mmol) in pyridine (4.0 mL) was added a solution of 8M aqueous potassium hydroxide (375 μL, 3.0 mmol) at room temperature. The mixture was stirred for 2 h, diluted with water and extracted with ethyl acetate. The ethyl acetate extract was washed successively with 1M aqueous NaOH (2x),0.5M aqueous HCl (1x), brine, dried over anhydrous MgSO4 and concentrated in vacuo. Chromatography over silica gel and eluted with toluene: ethyl acetate (10:1) afforded the title compound (590 mg, 81%) as a pale yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05604260 |
| Source dataset | uspto-grants-1997_02 |
| ORD ID | ord-f484bf81f4e64459b033c0d819875e04 |
| Source note | uspto-grants-1997_02 |