Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Butyl bromide | HCID 8002 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Magnesium | HCID 5462224 | — |
| Product | HCID 178448196 | HCID 178448196 | 80% |
Reaction Steps
Under argon atmosphere, into a 100 mL-volume flask equipped with a stirrer, a thermometer and a dropping funnel were placed 5.5 g (0.23 mol) of metallic magnesium and 20 ml of diethyl ether. And then, 3.0 g (21 mmol) of bromobutane was slowly dropped into the flask. Subsequently, 180 ml of diethyl ether and 25 g (0.18 mol) of bromobutane were slowly dropped into the flask, and the mixture was reacted while stirring at 40° C. for 2 hours. And then, 55 g (0.62 mol) of dioxane was added to the reaction solution, and the mixture was reacted while stirring at 40° C. for 2 hours. After the completion of the reaction, under argon atmosphere, the reaction solution was filtrated, and the filtrate was concentrated under reduced pressure. The resultant concentrate was heated and dried under vacuum, to provide 22 g of dibutyl magnesium. (Isolation yield: 80%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08871304B2 |
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| Source dataset | uspto-grants-2014_10 |
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| ORD ID | ord-ee1aa8b44c8141ddadf3b99777567f83 |
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| Source note | uspto-grants-2014_10 |
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