HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Methyl-2-butene → HCID 66682626, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Methyl-2-butene | HCID 10553 | — |
| Reactant | Sodium Chlorite | HCID 23668197 | — |
| Reactant | Sodium Phosphate, Monobasic, Dihydrate | HCID 23673460 | — |
| Reactant | HCID 86649568 | HCID 86649568 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 66682626 | HCID 66682626 | 109.5% |
Reaction Steps
Benzyl 5-{3-(2-Fluoro-4-formylphenoxy)-5-[(1S)-2-methoxy-1-methylethoxy]phenyl}-1H-pyrrole-2-carboxylate (6.33 g, 12.6 mmol) synthesized in Example (66d) was suspended in a mixed solvent of t-butanol (120 mL) and water (40 mL), and sodium dihydrogen phosphate dihydrate (8.86 g, 56.8 mmol) and 2-methyl-2-butene (12.05 mL, 113 mmol) were added. Under ice cooling, sodium chlorite (80%, 2.93 g, 25.9 mmol) was added slowly, and stirring was carried out at room temperature for 2 hours. Saturated brine (200 mL) was added, followed by extraction with dichloromethane (200 mL), and drying was carried out over anhydrous magnesium sulfate to afford the desired compound (7.17 g, yield ˜100%) as a pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08415359B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-bb8967a184734e018e89ef6bfe01a254 |
| Source note | uspto-grants-2013_04 |