HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → 1-{[2-(Trimethylsilyl)ethoxy]methyl}pyridin-4(1H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 2-Chloromethyl 2-(trimethylsilyl)ethyl ether | HCID 2724271 | — |
| Reactant | HCID 178418642 | HCID 178418642 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1-{[2-(Trimethylsilyl)ethoxy]methyl}pyridin-4(1H)-one | HCID 14005160 | — |
Reaction Steps
To a solution of 4-hydroxypyridine (3.0 g, 32 mmol) and trimethylsilylethoxymethyl chloride (5.5 mL, 32 mmol) in 30 mL of acetonitrile was added cesium carbonate (11 g, 34 mmol). After stirring at room temperature overnight, the reaction mixture was partitioned between brine (100 mL) and ethyl acetate (100 mL). The organic layer was separated and aqueous layer extracted with ethyl acetate (3×100 mL). The combined extracts were dried over anhydrous sodium sulfate, filtered, and concentrated to dryness to give the title compound contaminated with some O-alkylated product. 1H NMR (500 MHz, CD3OD): δ 7.92 (d, 2H), 6.49 (d, 2H), 5.28 (s, 2H), 3.62 (t, 2H), 0.96 (t, 2H), 0.024 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07576239B2 |
| Source dataset | uspto-grants-2009_08 |
| ORD ID | ord-b05a71cbcd304757ba309d5d710f74c9 |
| Source note | uspto-grants-2009_08 |