反应 #674376

反应方程式

4-bromo-2-fluorobenzoic acid

ethyl magnesium bromide

→

4-bromo-2-ethylbenzoic acid

溶剂

THF

THF

反应条件

后处理

1. 1
   其他the resultant reaction mixture
2. 2
   其他The reaction mixture was quenched with 2 N HCl
3. 3
   萃取extracted with EtOAc
4. 4
   干燥The combined EtOAc layer was dried over anhydrous Na2SO4
5. 5
   浓缩concentrated under reduced pressure

实验过程

To a stirred solution of 4-bromo-2-fluorobenzoic acid (2.0 g, 9.17 mmol) in THF (16 mL), was added 1.0 M ethyl magnesium bromide in THF (32 mL, 32.0 mmol) dropwise at 0° C. and the resultant reaction mixture was stirred at ambient temperature for 18 h. The reaction mixture was quenched with 2 N HCl and extracted with EtOAc. The combined EtOAc layer was dried over anhydrous Na2SO4 and concentrated under reduced pressure to afford crude 4-bromo-2-ethylbenzoic acid as a colorless liquid that was used in the next step without purification (0.4 g): 1H NMR (400 MHz, CDCl3) δ 7.64 (d, J=8.4 Hz, 1H), 7.47 (m, 1H), 7.43 (m, 1H), 2.95 (q, J=4.0 Hz, 2H), 1.32 (t, J=4.0 Hz, 3H); ESIMS m/z 228.97 ([M+H]+).

来源