HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 22054074, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Benzyl mercaptan | HCID 7509 | — |
| Reactant | HCID 22053958 | HCID 22053958 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22054074 | HCID 22054074 | — |
Reaction Steps
4-(4-Methylsulfonylamino-phenyl)-2-methylene-4-oxo-butyric acid (800 mg, 2.83 mmol) was dissolved in DMF (5 mL). Benzyl mercaptan (0.5 mL, 4.25 mmol) and DMAP (200 mg, 1.6 mmol) were added. The mixture was stirred at ambient temperature for 16 hours. Methanol (200 mL) was added and, under vigorous stirring, a saturated aqueous solution of Oxone® (15 g, 24.4 mmol) was added in one portion. Stirring was continued for 2 hours. Methanol was removed under vacuum and the aqueous residue was diluted with 100 mL water. The crystallized product, 4-(4-Methylsulfonylamino-phenyl)-4-oxo-2-benzylsulfonylmethyl-butyric acid (380 mg), was filtered, washed with water, and dried under vacuum.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07064123B1 |
| Source dataset | uspto-grants-2006_06 |
| ORD ID | ord-f17cd9bccd884373aff76b8895986225 |
| Source note | uspto-grants-2006_06 |