反应详情

In a three-necked flask, a solution of 1-bromobutane (34.25 g, 250 mmol) in diethyl oxide was added on magnesium (7.3 g, 300 mmol) covered with dry diethyl oxide. When the addition was completed, the mixture was refluxed during one hour. This solution was then added to triphenyltin chloride (42.6 g, 110 mmol) in 150 mL of diethyl oxide and refluxed for 3 hours. The mixture was hydrolysed with a minimum of water, washed with a saturated aqueous solution of sodium chloride, dried over magnesium sulphate and concentrated. Crystallization of the crude product in methanol gave a white solid (32.3 g, 93 mmol).

1. additionWhen the addition
2. temperaturethe mixture was refluxed during one hour
3. temperaturerefluxed for 3 hours
4. washwashed with a saturated aqueous solution of sodium chloride
5. dry with materialdried over magnesium sulphate
6. concentrationconcentrated
7. customCrystallization of the crude product in methanol