HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 136163974, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 667398-46-1 | HCID 135532669 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 136163974 | HCID 136163974 | — |
Reaction Steps
5-(hydroxymethyl)-4-(1H-imidazol-2-yl)-2-methylpyridin-3-ol (1.03 g, 5.0 mmol) was suspended in DMF (50 mL) and methyl iodide (0.31 mL, 5 mmol) was added at rt. The reaction mixture was stirred over a period of 19 h and a further portion of methyl iodide (0.125 mL, 2 mmol) was added and stirred over a period of 23 h. Aq. K2CO3 solution (10 mL) and water (50 mL) was added and extracted with ethyl acetate (2×50 mL). Combined organic layers were dried over MgSO4 (10 g) and evaporated to a volume of 20 mL. After 3 days at room temperature, the crystallized product was filtered off and dried to give (600 mg) the title compound as a light beige solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09428533B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-3c160a64e43542dea37748f9fb967dcc |
| Source note | uspto-grants-2016_08 |