HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 11807573, compound → HCID 10945871, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 11807573 | HCID 11807573 | — |
| Reactant | Sodium Hypochlorite | HCID 23665760 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10945871 | HCID 10945871 | 77% |
Reaction Steps
To the pre-cooled solution of 0.55 M NaOCl (55 mL, 30.0 mmol) and of 0.05 M Na2HPO4 (21.5 mL) at 0° C., (2R)-2-dimethoxymethyl-2-methyl-6-nitro-2H-1-benzopyran n(2 g, 7.5 mmol) and (R, R) Jacobson's catalyst (477.5 mg, 0.75 mmol) in CH2Cl2 (10 mL) was added. The reaction mixture was stirred at rt for 8 hr and then filtered through Celite to remove the jacobson's catalyst. The layer was separated and the organic layer was washed with brine, dried (Na2SO4), filtered, then concentrated under reduced pressure. The residue was purified by silicagel column chromatography (n-hexane:ethyl acetate=4:1) to give the desired compound (1.64 g, 77%) as a light yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06413983B1 |
| Source dataset | uspto-grants-2002_07 |
| ORD ID | ord-b115c09af05e48119dcee204ef2d367f |
| Source note | uspto-grants-2002_07 |