Homoallyl bromide → HCID 178448195、化合物

A mixture of magnesium turnings (0.5 g, 0.02 mole) and dry THF (5 mL) were placed in a dry, three-necked round-bottomed flask under argon. To this was added dropwise a solution of 2.3 g (0.7 mole) of 4-bromobutene in 5 mL of dry THF. After about 1/3 of the bromobutene was added, the reaction had not initiated. Two drops of dibromoethane was added and the reaction heated to reflux until Grignard formation was initiated. Heating was stopped and the remainder of the halide was added dropwise to maintain a gentle reflux. After all of the halide was added, the reaction was heated briefly then treated with 1.5 g (0.017 mole) of dioxane with stirring. An immediate white precipitate was formed. This suspension was used in the next step without further purification.

1. temperaturethe reaction heated
2. temperatureto reflux until Grignard formation
3. temperatureHeating
4. temperatureto maintain a gentle reflux
5. temperaturethe reaction was heated briefly
6. customAn immediate white precipitate was formed
7. customThis suspension was used in the next step without further purification

ORDレコード

ord-4be068d7828742fc8009d0367e22ccd0

出典データセット

uspto-grants-1988_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04772755