HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 71666040, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | HCID 117701775 | HCID 117701775 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 71666040 | HCID 71666040 | 54% |
Reaction Steps
N-Bromosuccinimide (171 mg, 0.96 mmol) was added to a solution of 7-hydroxy-3-methyl-2-(1-propanoylpiperidin-4-yl)-4H-chromen-4-one (304 mg, 0.96 mmol) obtained in Example 31-3 in N,N-dimethylformamide (5 mL), and the mixture was stirred at room temperature for 5 hours. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was washed with water and saturated brine and dried over anhydrous sodium sulfate, and then the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography (dichloromethane/methanol=98/2→67/33) to obtain 204 mg of the title compound (yield: 54%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09221811B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-f3bf4c998e2745f7b34d8465068d0b11 |
| Source note | uspto-grants-2015_12 |