HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 117701563, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2-Methyl-2-butene | HCID 10553 | — |
| Reactant | Sodium Chlorite | HCID 23668197 | — |
| Reactant | Sodium Phosphate, Monobasic, Dihydrate | HCID 23673460 | — |
| Reactant | HCID 117701716 | HCID 117701716 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | HCID 117701563 | HCID 117701563 | 98.4% |
Reaction Steps
To a mixture composed of 7-(benzyloxy)-3-methyl-4-oxo-2-(1-propanoylpiperidin-4-yl)-4H-chromene-8-carbaldehyde (400 mg, 0.92 mmol) obtained in Example 34-2, tert-butyl alcohol (8 mL), water (8 mL), 2-methyl-2-butene (8 mL), and sodium dihydrogen phosphate dihydrate (864 mg, 5.54 mmol), 80% sodium chlorite (313 mg, 2.77 mmol) was added under cooling with ice, and then the mixture was brought back to room temperature and stirred for 19 hours. A 0.2 N aqueous hydrochloric acid solution (20 mL) was added to the reaction solution, and then the organic solvent was distilled off under reduced pressure. The resulting solid was collected by filtration to obtain 407 mg of the title compound (yield: 95%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09221811B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-5f4ed039cece49dda8a6ab7604d0e85f |
| Source note | uspto-grants-2015_12 |