HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl bromoacetate → Ethyl 2-(2-oxopyridin-1-YL)acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl bromoacetate | HCID 7748 | — |
| Reactant | 2-Pyridone | HCID 8871 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | 2(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl- | HCID 81646 | — |
| Product | Ethyl 2-(2-oxopyridin-1-YL)acetate | HCID 9497629 | 76.2% |
Reaction Steps
To a suspension of 60% sodium hydride dispersion in mineral oil (220 mg, 5.5 mmol) in cold (0° C.) THF is added 2-pyridone (475 mg, 5.0 mmol) in THF (4 mL) and DMPU (2 mL) followed by ethyl bromoacetate (0.556 mL, 5.0 mmol), and the reaction is stirred at RT for 1 h. The reaction is quenched with water, and extracted with EtOAc. The organic layer is separated, evaporated, and the residue purified by chromatography on silica gel; elution with EtOAC:dichloromethane:heptane (50:30:20) gives 690 mg of the product 425. 1H NMR (CDCl3) δ 7.35 (m, 1H), 7.21 (d, 1H), 6.57 (d, 1H), 6.19 (t, 1H), 4.62 (s, 2H), 4.23 (q, 2H), 1.28 (t, 3H); MS: m/z 182 (M++1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07326792B2 |
| Source dataset | uspto-grants-2008_02 |
| ORD ID | ord-85c52524d0204443ac20b624a94d3759 |
| Source note | uspto-grants-2008_02 |