反应详情

温度

62.5 °C

A solution of bromobutane (0.98 mol) in 28 grams of THF is heated to 60-65° C. A warm solution of CpMgCl in THF (1.0 mol) as produced in Example 1 is added to the bromobutane solution while maintaining a pot temperature between 60-65° C. After the addition and the consequent reaction are complete by GC analysis, the reaction mixture is cooled to ambient temperature, 25% by weight of aqueous acetic acid is added, and the organic layer is separated, washed with 10% by weight of aqueous sodium carbonate, and dried over anhydrous sodium sulfate. The organic layer is filtered, and fractionally distilled under reduced pressure to recover 70 to 80% yield of n-butyl cyclopentadiene.

1. additionAfter the addition
2. customthe consequent reaction
3. temperaturethe reaction mixture is cooled to ambient temperature
4. customthe organic layer is separated
5. washwashed with 10% by weight of aqueous sodium carbonate
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationThe organic layer is filtered
8. distillationfractionally distilled under reduced pressure