HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → 1-(4-Bromo-3-fluorophenyl)-2,2-diethoxyethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | 2-fluoro-N-[(2R)-2-hydroxypropyl]-4-[7-(quinolin-6-ylmethyl)imidazo[1,2-b][1,2,4]triazin-2-yl]benzamide | HCID 53374318 | — |
| Reactant | Ethylorthoformate | HCID 53630039 | — |
| Reactant | 1-(4-Bromo-3-fluorophenyl)-2,2-dihydroxyethanone | HCID 57516521 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 1-(4-Bromo-3-fluorophenyl)-2,2-diethoxyethanone | HCID 57516522 | — |
Reaction Steps
To a mixture of 1-(4-bromo-3-fluorophenyl)-2,2-dihydroxyethanone and 4-bromo-3-fluorophenyl)(oxo)acetaldehyde (crude product from Step 3, 7.0 g, 28 mmol) in toluene (50 mL) was added ethyl orthoformate (12 mL, 70 mmol) and p-toluenesulfonic acid (200 mg, 1 mmol). The reaction mixture was refluxed for 4 h. The reaction mixture was cooled to RT, diluted with ethyl acetate, washed with aqueous sodium bicarbonate, water, brine, and dried over magnesium sulfate. Concentration under reduced pressure gave the desired product which was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08487096B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-099f00c91bb941e4ab42dba41f944f2c |
| Source note | uspto-grants-2013_07 |