HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 178494189, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Triacetoxyperiodinane | HCID 159087 | — |
| Reactant | HCID 178432606 | HCID 178432606 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178494189 | HCID 178494189 | 45.3% |
Reaction Steps
To a stirred suspension of 3-(5-(hydroxymethyl)-4-methyl-1H-imidazol-2-yl)-4-iodopyridin-2(1H)-one (0.020 g, 0.0579 mmol) in dichloromethane (2 mL) was added the Dess-Martin reagent (0.049 g, 0.1158 mmol) at room temperature. The reaction became clear after 5 minutes of stirring. Ethyl acetate was added and the reaction was washed with 5% aqueous Na2S2O3.5H2O, saturated aqueous sodium bicarbonate and brine. The organic layer was driede over anhydrous magnesium sulfate, filtered and concentrated. The residue was purified on silica gel chromatography (ethyl acetate) to give the title material (0.009 g, 45%). 1H NMR (400 MHz, Acetone-d6) δ (ppm): 2.47 (s, 3H) 3.72 (s, 3H) 7.42-7.50 (m, 1H) 7.78 (s, 1H) 9.81 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07470713B2 |
| Source dataset | uspto-grants-2008_12 |
| ORD ID | ord-6d602de9fadd49b9b56df4f9e17bf8a5 |
| Source note | uspto-grants-2008_12 |