反应 #595370

反应方程式

4-bromo-2-fluoro-5-methylbenzoic acid

SOCl2

CH3OH

→

title compound

methyl 4-bromo-2-fluoro-5-methylbenzoate

反应条件

后处理

1. 1
   其他The solvent was removed in vacuo
2. 2
   workup.ADDITIONthe residue was diluted with EtOAc
3. 3
   洗涤washed with H2O, brine
4. 4
   干燥dried over anhydrous Na2SO4
5. 5
   浓缩concentrated
6. 6
   洗涤The resulting crude solid was washed with PE

实验过程

To a solution of 4-bromo-2-fluoro-5-methylbenzoic acid (i-2a) (1.87 g, 8 mmol) in CH3OH (50 mL) at 0° C. was added SOCl2 (6 mL, 80 mmol) dropwise. Then the mixture was heated to 80° C. for 2 h. The solvent was removed in vacuo and the residue was diluted with EtOAc and washed with H2O, brine, dried over anhydrous Na2SO4, and concentrated. The resulting crude solid was washed with PE to give the title compound as a yellow solid. 1H NMR (400 MHz, CDCl3) δ 7.80 (1H, d), 7.37 (1H, d), 3.92 (3H, s), 2.39 (3H, s).

来源