反应详情

A mixture of Mg turnings (0.6 g, 24 mmole), [(5-bromo-1-pentyl)oxy]-(1,1-dimethylethyl)dimethylsilane (0.5 mL), and MeMgBr (0.2 mL, 3 M) in dry OEt2 (5 mL) was stirred and heated to reflux for 5 minutes under an inert atmosphere. A solution of [(5-bromo-10-pentyl)oxy](1,1-dimethyl-ethyl)dimethylsilane (5.62 g, 20 mmole) and MeMgBr (0.2 mL, 3 M) in dry OEt2 (20 mL) was added dropwise at a rate to maintain a gentle, unassisted reflux. After addition was complete, the reaction was heated at reflux for 45 minutes. The solution of Grignard reagent was then cooled and used immediately in the next reaction.

1. temperatureheated
2. temperatureto reflux for 5 minutes under an inert atmosphere
3. temperatureto maintain a gentle, unassisted reflux
4. additionAfter addition
5. temperaturethe reaction was heated
6. temperatureat reflux for 45 minutes
7. customused immediately in the next reaction