反应详情

温度

80 °C

A mixture of ethyl(3-bromophenyl)acetate (0.3 g, 1.24 mmol) and tetrabutylammonium fluoride hydrate (0.97 g, 3.72 mmol), was treated with PdCl2(PPh3)2 (26 mg, 0.037 mmol; 3 mole %) and 1-pentyne (367 μL, 3.72 mmol) in a sealed tube. The tube was heated at 80° C. for 2 h. The mixture was treated with water, and was extracted with diethyl ether. The organic extract was dried over sodium sulfate, filtered and evaporated in vacuo to give the crude product. Purification on a Biotage™ 25 M column (silica), eluting with ethyl acetate/hexane 0:1 to 2:98, gave ethyl (3-(pentyne-1-yl)phenyl)acetate as a pale yellow oil (0.23 g, 79%).

1. extractionwas extracted with diethyl ether
2. extractionThe organic extract
3. dry with materialwas dried over sodium sulfate
4. filtrationfiltered
5. customevaporated in vacuo
6. customto give the crude product
7. customPurification on a Biotage™ 25 M column (silica)
8. washeluting with ethyl acetate/hexane 0:1 to 2:98