反応 #54992

反応方程式

4-ethynyl-4'-fluorobiphenyl

ethyl magnesium bromide

ethylene oxide

→

4-(4'-Fluoro-4-biphenylyl)-3-butyn-1-oxymagnesium bromide

溶媒

THF

THF

THF

反応条件

後処理

1. 1
   workup.ADDITIONto which is added 100 ml
2. 2
   その他After subsidance of the exothermic reaction
3. 3
   温度the mixture is heated
4. 4
   温度under reflux for 1 hour

実験手順

19.6 g. of 4-ethynyl-4'-fluorobiphenyl in 200 ml. THF is converted with an excess of ethyl magnesium bromide to the Grignard compound, to which is added 100 ml. of THF and then a solution of 5 g. of ethylene oxide in 10 ml. of THF. After subsidance of the exothermic reaction, the mixture is heated under reflux for 1 hour. 4-(4'-Fluoro-4-biphenylyl)-3-butyn-1-oxymagnesium bromide is thereby formed in situ. To this is added 150 ml. of 1 N hydrochloric acid. After stirring for 20 minutes at 20° and the usual work up, 4-(4'-fluoro-4-biphenylyl)-3-butyn-1-ol, m.p. 134°, is obtained.

出典