HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Thiosulfate → HCID 68806008, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | HCID 68807404 | HCID 68807404 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68806008 | HCID 68806008 | — |
Reaction Steps
2-(3-Fluoro-2′-methylsulfanyl-biphenyl-4-ylcarbamoyl)-pyrrolidine-1-carboxylic acid tert-butyl ester (1.2 g, 2.8 mmol) was dissolved in 30 mL EtOAc, added m-chloroperoxybenzoic acid (3.2 g, 11 mmol) in one portion and stirred at ambient temperature for 3 hours. A 10% aqueous solution (50 mL) of Na2S2O3 was added to the vigorously stirring reaction in order to quench peroxide. After 30 minutes the solution was diluted with 100 mL EtOAc, separated layers, washed organics with sat. NaHCO3 (3×100 mL), brine, dried with MgSO4, filtered and concentrated. Purified on a silica gel column eluted with 50% EtOAc in hexanes. Combined and concentrated pure fractions to yield title compound as a yellow foam. (1.01 g, 78%) APCI (AP−): 461.1 (M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07407974B2 |
| Source dataset | uspto-grants-2008_08 |
| ORD ID | ord-04bfaae29b224ec79730e05602f9d70a |
| Source note | uspto-grants-2008_08 |