HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cornforth reagent → Toluene-4-sulfonic acid 5-acetyl-1H-pyrazol-3-yl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cornforth reagent | HCID 2724130 | — |
| Reactant | toluene-4-sulfonic acid 5-[(S)-l-hydroxyethyl]-1H-pyrazol-3-yl ester | HCID 87418248 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Toluene-4-sulfonic acid 5-acetyl-1H-pyrazol-3-yl ester | HCID 87418291 | 85% |
Reaction Steps
To toluene-4-sulfonic acid 5-[(S)-1-hydroxyethyl]-1H-pyrazol-3-yl ester (6.09 g, 21.6 mmol) in anhydrous dichloromethane (180 ml) was added pyridinium dichromate (9.74 g, 25.9 mmol) and the resulting slurry was stirred at room temperature for 17.6 h. The mixture was poured directly onto a column of silica gel, which was eluted with ethyl acetate to yield 5.13 g (85%) of the title compound as a whitish solid: 1H NMR (360 MHz, DMSO-d6) δ 2.43 (3H, s), 2.45 (3H, s), 6.78 (1H, s), 7.49 (2H, d, J=8.2 Hz), 7.80 (2H, d, J=8.3 Hz), 13.72 (1H, s); MS (ES+) m/e 281 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06872720B2 |
| Source dataset | uspto-grants-2005_03 |
| ORD ID | ord-f7d9f9776713465383fb12c31cc60c67 |
| Source note | uspto-grants-2005_03 |