HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67003455, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 67003422 | HCID 67003422 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 67003455 | HCID 67003455 | — |
Reaction Steps
A solution of Example 47A (0.074 g, 0.127 mmol) in methanol (1.5 mL) and 2 M aqueous sodium hydroxide solution (0.317 mL, 0.633 mmol) was heated at 75° C. for 15 minutes. The reaction was cooled to ambient temperature, and the pH adjusted to ˜7 with 10% aqueous HCl solution. The resulting suspension was extracted with ethyl acetate. The aqueous layer was extracted with additional ethyl acetate. The combined organic layers were washed with brine, dried over anhydrous sodium sulfate, filtered, and concentrated. The concentrate was purified by flash chromatography on a silica gel column with a gradient of 0% to 3% methanol in dichloromethane to provide the title compound. ESI(+) m/z 429.9 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08691810B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-d00a38b567ea48e289367e837fc8a3b2 |
| Source note | uspto-grants-2014_04 |