반응 #1252936

반응 방정식

trimethylsilyl chloride

magnesium ethyl bromide

NH4Cl

compound

1-bromo-3-ethynylbenzene

→

3-(trimethylsilylethynyl)bromobenzene

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.WAITThen, over 2 minutes
2. 2
   온도without cooling
3. 3
   workup.STIRRINGwith stirring for 30 minutes at 25° C
4. 4
   추출was extracted with ether
5. 5
   기타dried
6. 6
   여과filtered
7. 7
   농축the filtrate was concentrated to dryness
8. 8
   workup.DISTILLATIONby distilling under reduced pressure

실험 절차

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.

출처