HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 86755954, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | (1-Bromoethyl)benzene | HCID 11454 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 86755953 | HCID 86755953 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 86755954 | HCID 86755954 | 91.3% |
Reaction Steps
To a mixture of 0.25 g (1 mmol) of 5-(2-hydroxyiminomethyl-α-methoxybenzyl)-3-methylisoxazole, 3 ml of N,N-dimethylformamide and 0.24 g (1.3 mmol) of α-methylbenzyl bromide was added 0.05 g (1.3 mmol) of 60% sodium hydride under ice-cooling and stirred at the same temperature for 3 hours. After completion of the reaction, 100 ml of ether was added and washed twice with 80 ml of brine. The ether layer was dried over anhydrous magnesium and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (ethyl acetate/n-hexane) to give 5-[α-methoxy-2-(4-phenyl-2-aza-3-oxa-1-pentenyl)benzyl]-3-methylisoxazole (0.32 g, 91.3%) as colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06136837 |
| Source dataset | uspto-grants-2000_10 |
| ORD ID | ord-cb5d8fc3a58444bfb0a038742b892484 |
| Source note | uspto-grants-2000_10 |