HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86610528, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | HCID 68419954 | HCID 68419954 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86610528 | HCID 86610528 | 89.7% |
Reaction Steps
Methyl 3,5-bis(methoxymethoxy)-2-(4-methoxybenzoyl)phenylacetate (490 mg, 1.2 mmol) obtained in Example 134, Step 2 was dissolved in N,N-dimethylformamide (10 mL), and N-bromosuccinimide (220 mg, 1.2 mmol) was added thereto, followed by stirring at room temperature for 3 hours. To the reaction mixture was added water for liquid separation, and the aqueous layer was extracted with ethyl acetate. The organic layers were combined, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/4-1/1) to obtain methyl 3,5-bis(methoxymethoxy)-2-bromo-6-(4-methoxybenzoyl)phenylacetate (520 mg, 89%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07538224B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-0614d7bb0d9f4d50ba6840953ca25d86 |
| Source note | uspto-grants-2009_05 |