HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 2-(4,6-Dichloro-1,5-naphthyridin-3-yl)-2-oxoethyl acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2-Chloro-1-(4,6-dichloro-1,5-naphthyridin-3-yl)ethanone | HCID 89705477 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | 2-(4,6-Dichloro-1,5-naphthyridin-3-yl)-2-oxoethyl acetate | HCID 89705165 | 42% |
Reaction Steps
To a solution of acetic acid (0.32 mL, 5.5 mmol) and N,N-diisopropylethylamine (0.87 mL, 5.0 mmol) in acetone (20 mL) was added 2-chloro-1-(4,6-dichloro-1,5-naphthyridin-3-yl)ethanone (0.26 g, 0.96 mmol) and the reaction mixture was stirred at room temperature for 4 h. The reaction mixture was diluted with satd. aq. sodium bicarbonate and extracted with dichloromethane. The combined organic layers were dried over anhydrous sodium sulfate, filtered and the filtrate was concentrated. The residue was purified by column chromatography (silica, dichloromethane/ethyl acetate) to afford the desired product (0.12 g, 42%) as a white solid. ESI MS m/z 299 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09345709B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-44bc67d9ed494a889a07d9e9fc48149e |
| Source note | uspto-grants-2016_05 |