HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 118114006, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 5-(chloromethyl)-2-methylpyridine hydrochloride | HCID 12214339 | — |
| Reactant | HCID 15713917 | HCID 15713917 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 118114006 | HCID 118114006 | 106.2% |
Reaction Steps
To a stirred solution of tert-butyl 4-hydroxy-3-methoxybenzylcarbamate (21.02 g, 82.99 mmol) in acetonitrile (250 mL) was added potassium carbonate (30.61 g, 221.5 mmol) and 5-(chloromethyl)-2-methylpyridine hydrochloride (16.25 g, 91.29 mmol). The resulting mixture was heated to reflux. After 63 h, the brown suspension was allowed to cool to room temperature and was diluted with water (1000 mL). The mixture was extracted with dichloromethane (3×250 mL). The combined organic phases were dried over magnesium sulfate, filtered, and concentrated to provide 31.59 g (>100%) of tert-butyl 3-methoxy-4-((6-methylpyridin-3-yl)methoxy)benzylcarbamate as a brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09067914B1 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-7eabc66439ad4ba0926de2711453a7d3 |
| Source note | uspto-grants-2015_06 |