HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 178500506, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | HCID 54499564 | HCID 54499564 | — |
| Reactant | Methyl 2-(2-bromophenyl)-3-oxobutanoate | HCID 82306029 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178500506 | HCID 178500506 | — |
Reaction Steps
To a solution of 1-(1,4-dioxan-2-yl)ethanamine (2.5 g, 19 mmol) in methanol (100 mL) was added methyl 2-(2-bromophenyl)-3-oxobutanoate (5.4 g, 20 mmol) and acetic acid (1.8 g, 30 mmol). The resulting reaction system was warm to reflux and allowed to stir overnight. The reaction mixture was concentrated and purified by column chromatographed on silica gel (eluted: dichloromethane/methanol 50:1→20:1→5:1) the title compound (1 g, 14%) as a brown solid. LCMS (M+H+) m/z: calcd. 383.07. found 384.9.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09371331B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-9cf8e57c4e0c419c9c3babe12dfe25d4 |
| Source note | uspto-grants-2016_06 |