HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 12112580, compound → HCID 12112584, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 12112580 | HCID 12112580 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 12112584 | HCID 12112584 | 72.2% |
Reaction Steps
A aqueous solution (100 ml) of OXONE (trade mark) (891 mg) was added dropwise to a solution of the compound prepared in Example 3(2) (1.0 g) in tetrahydrofuran (200 ml) over a period of 30 minutes at −2˜−3° C., and the resultant solution was stirred for 10 minutes at 0° C. Ice water was added to the reaction solution, and the resultant solution was extracted with ethyl acetate, and the extract was washed with water and a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography (chloroform:methanol=50:1→10:1) to give the title compound (750 mg) having the following physical data.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06821994B2 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-bb6cb6c0df28464e8a8f0b968b4ae3b8 |
| Source note | uspto-grants-2004_11 |