反应详情

温度

25 °C

Under an inert atmosphere, 9.5 g of the compound of Step A were introduced into 100 g of tetrahydrofuran, and at 25° C.±3° C., over 15 minutes, 69 ml of a 0.8M solution of magnesium ethyl bromide were added, with stirring for 15 minutes at 25° C. Then, over 2 minutes and without cooling, 8 ml of trimethylsilyl chloride were added with stirring for 30 minutes at 25° C. The reaction mixture was poured into a 2M aqueous solution of NH4Cl and was extracted with ether, dried, filtered, and the filtrate was concentrated to dryness by distilling under reduced pressure then rectified to obtain 12.1 g of 3-(trimethylsilylethynyl)bromobenzene with a boiling point at 0.05 mm/Hg=78° to 84° C.

1. waitThen, over 2 minutes
2. temperaturewithout cooling
3. stirringwith stirring for 30 minutes at 25° C
4. extractionwas extracted with ether
5. customdried
6. filtrationfiltered
7. concentrationthe filtrate was concentrated to dryness
8. distillationby distilling under reduced pressure