Activation of Mg Metal for Safe Formation of Grignard Reagents on Plant Scale
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- 作者：Ulf Tilstam and Hilmar Weinmann
- 刊名：Organic Process Research & Development
- 出版年：2002
- 出版时间：November 2002
- 年：2002
- 卷：6
- 期：6
- 页码：906 - 910
- 全文大小：78K
- 年卷期：v.6,no.6(November 2002)
- ISSN：1520-586X
文摘
A general and reliable method for the activation of magnesiummetal for the formation of various kinds of Grignard reagentshas been developed. Utilizing diisobutylaluminum hydride(DIBAH) for the activation of the surface and drying of thereaction mixture the initiation of the Grignard reagent formation can be performed at or below 20 
C for aryl Grignardreagents. For alkyl bromides it is possible to activate themagnesium turnings at even lower temperatures. As thetemperature is well below the boiling point of THF, it is possibleto detect the initiation of the reaction through the temperaturerise. The initiation method was found to be reliable also undervery diluted reaction conditions as long as the reaction mixturewas stirred. We have also shown that with this method it ispossible to manufacture Grignard reagents well below theboiling point of THF.
C for aryl Grignardreagents. For alkyl bromides it is possible to activate themagnesium turnings at even lower temperatures. As thetemperature is well below the boiling point of THF, it is possibleto detect the initiation of the reaction through the temperaturerise. The initiation method was found to be reliable also undervery diluted reaction conditions as long as the reaction mixturewas stirred. We have also shown that with this method it ispossible to manufacture Grignard reagents well below theboiling point of THF.