Diethyl Ether → HCID 178448196, compound

Temperature

40 °C

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%)

1. customUnder argon atmosphere, into a 100 mL-volume flask equipped with a stirrer
2. customthe mixture was reacted
3. customthe mixture was reacted
4. stirringwhile stirring at 40° C. for 2 hours
5. customAfter the completion of the reaction
6. filtrationunder argon atmosphere, the reaction solution was filtrated
7. concentrationthe filtrate was concentrated under reduced pressure
8. concentrationThe resultant concentrate
9. temperaturewas heated
10. customdried under vacuum

ORD record

ord-ee1aa8b44c8141ddadf3b99777567f83

Source dataset

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08871304B2