HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → Methyl 2-methoxy-5-(t-butyldimethylsilyloxy)benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl 5-((tert-butyldimethylsilyl)oxy)-2-hydroxybenzoate | HCID 18465044 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Ethyl acetate hexane | HCID 21226206 | — |
| Product | Methyl 2-methoxy-5-(t-butyldimethylsilyloxy)benzoate | HCID 18464864 | — |
Reaction Steps
Combine methyl 2-hydroxy-5-(t-butyldimethylsilyloxy)benzoate (14.2 g, 50.2 mmol), potassium carbonate (13.88 g, 100.4 mmol), and methyl iodide (20 mL, 321 mmol) in acetone (125 mL). Heat to reflux. After 17 hours, add methyl iodide (10 mL). After 23 hours, cool the reaction mixture to ambient temperature and add diethyl ether (600 mL), filter, and evaporate the filtrate in vacuo to give a residue. Chromatograph the residue on silica gel eluting with 10% ethyl acetate/hexane to give methyl 2-methoxy-5-(t-butyldimethylsilyloxy)benzoate. Rf=0.39 (silica gel, 5% ethyl acetate/hexane).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06423704B1 |
| Source dataset | uspto-grants-2002_07 |
| ORD ID | ord-9ded7963a0b646b2a2647fc38d708dee |
| Source note | uspto-grants-2002_07 |