HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → HCID 86761914, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| Reactant | HCID 86761915 | HCID 86761915 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86761914 | HCID 86761914 | 42.4% |
Reaction Steps
The compound (130 mg, 0.165 mmol) obtained in Example 87b was dissolved in a mixed solvent of 1,4-dioxane (1.6 mL) and methanol (1.6 mL), a 4 N hydrochloric acid-dioxane solution (0.412 mL, 1.65 mmol) was added, and the mixture was stirred at room temperature for 4 hours. After the reaction was completed, a saturated aqueous sodium hydrogencarbonate solution was added, the mixture was extracted (×3) with methylene chloride, and the resulting organic layer was dried with anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the resulting residue was purified by NH silica gel column chromatography to give the title compound (48 mg; yield, 42%) as a colorless oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08476253B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-4d9adaa65527409f929ffec46b82989c |
| Source note | uspto-grants-2013_07 |