HuagongsheHuagongshe Chemistry Print Report · For research reference only
m-Chloroperbenzoic acid → HCID 22712131, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | HCID 22712074 | HCID 22712074 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22712131 | HCID 22712131 | 65.3% |
Reaction Steps
To a solution of 3,5-dichloro-2-fluoro-4-(3-isopropyl-4-hydroxyphenylthio)-6-hydroxycarbonylmethylaminopyridine (25 mg, 0.06 mmol) in CH2Cl2 (1.5 mL) was added 3-chloroperoxy-benzoic acid (11 mg). The mixture was left to stir overnight (ca. 15 h) at ambient room temperature. The product was extracted with EtOAc (25 mL). The organic extract was washed with brine (25 mL), dried (Na2SO4), filtered and concentrated in vacuo. The isolated crude product was purified by preparative HPLC (from 50% B to 100% B for 10 min, Solvent A=90% H2O-10% MeOH-0.1% TFA Solvent B=10% MeOH-90% H2O-0.1% TFA, at 20 mL/min using column YMC ODS S5 20×100 mm) to afford 16.5 mg (64%) of title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06747048B2 |
| Source dataset | uspto-grants-2004_06 |
| ORD ID | ord-a829e5220dcd4129ad730dc372fe40ef |
| Source note | uspto-grants-2004_06 |