HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 9816197, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 9816246 | HCID 9816246 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 9816197 | HCID 9816197 | 82.9% |
Reaction Steps
To a solution of N-(2-hydroxy-1,1-dimethylpropyl)-2,4-difluorobenzamide obtained in Example 33 (0.30 g, 1.2 mmol) and triethylamine (0.37 g, 3.7 mmol) in DMSO (3 ml) was added pyridine sulfur trioxide complex (0.59 g, 3.7 mmol) portionwise and stirred at room temperature for 3 hours. The reaction mixture was added to a mixture of ice and water and extracted with ethyl acetate. The extract was washed with 1N hydrochloric acid, saturated aqueous NaHCO3 and brine, successively dried over Na2SO4 and concentrated under a reduced pressure. The residue was crystallized from hexane/ethyl acetate to give the title compound (0.24 g; 81%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06936736B2 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-28919325596b47d9b18815170a447f56 |
| Source note | uspto-grants-2005_08 |